EP4258884A1 - Antimicrobial liquid composition and use thereof as a preservative activator in cosmetic products - Google Patents

Antimicrobial liquid composition and use thereof as a preservative activator in cosmetic products

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Publication number
EP4258884A1
EP4258884A1 EP21824287.3A EP21824287A EP4258884A1 EP 4258884 A1 EP4258884 A1 EP 4258884A1 EP 21824287 A EP21824287 A EP 21824287A EP 4258884 A1 EP4258884 A1 EP 4258884A1
Authority
EP
European Patent Office
Prior art keywords
acid
antimicrobial
chosen
weight
salts
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
EP21824287.3A
Other languages
German (de)
French (fr)
Inventor
Géraldine LOUVET-POMMIER
Léon Mentink
Daniel Wils
Nicolas Tesse
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Roquette Freres SA
Original Assignee
Roquette Freres SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority claimed from FR2013020A external-priority patent/FR3117310B1/en
Application filed by Roquette Freres SA filed Critical Roquette Freres SA
Publication of EP4258884A1 publication Critical patent/EP4258884A1/en
Pending legal-status Critical Current

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Classifications

    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
    • A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/02—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms
    • A01N43/04—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom
    • A01N43/14—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings
    • A01N43/16—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one or more oxygen or sulfur atoms as the only ring hetero atoms with one hetero atom six-membered rings with oxygen as the ring hetero atom
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
    • A01N65/40—Liliopsida [monocotyledons]
    • A01N65/44—Poaceae or Gramineae [Grass family], e.g. bamboo, lemon grass or citronella grass
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P3/00—Fungicides
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/02—Cosmetics or similar toiletry preparations characterised by special physical form
    • A61K8/04—Dispersions; Emulsions
    • A61K8/06—Emulsions
    • A61K8/062—Oil-in-water emulsions
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34—Alcohols
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365—Hydroxycarboxylic acids; Ketocarboxylic acids
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36—Carboxylic acids; Salts or anhydrides thereof
    • A61K8/368—Carboxylic acids; Salts or anhydrides thereof with carboxyl groups directly bound to carbon atoms of aromatic rings
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/60—Sugars; Derivatives thereof
    • A61K8/602—Glycosides, e.g. rutin
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00—Cosmetics or similar toiletry preparations
    • A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
    • A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
    • A61K8/9783—Angiosperms [Magnoliophyta]
    • A61K8/9794—Liliopsida [monocotyledons]
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q5/00—Preparations for care of the hair
    • A61Q5/02—Preparations for cleaning the hair
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
    • A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
    • A61K2800/52—Stabilizers
    • A61K2800/524—Preservatives

Definitions

  • the invention relates to the field of the preservation of cosmetic products, and more specifically to the field of activators of preservatives for cosmetic products.
  • preservative activator In order to obtain a preservative effect.
  • preservative activators are not preservatives listed as such, but have activities, in particular antimicrobial, which supplement or increase the antimicrobial activity of the preservatives.
  • Lonza patent WO 2014/014416 teaches antimicrobial compositions composed of a preservative active ingredient and a potentiator of said active ingredient.
  • the preservative active can be chosen from a multitude of compounds, ranging from cinnamaldehyde to sorbic acid or benzoic acid, and essential oils of wintergreen or lemongrass.
  • the potentiator can be chosen from erythorbic acid or gluconic acid, or their salts. Regarding gluconic acid, its cyclic form, known as gluconolactone, is preferred.
  • Lemongrass oil is cited in this application, and the antibacterial activity data presented show that this essential oil does not have sufficient activity to act as a preservative or preservative activator. Many additives are mentioned in this application, including solubilizers, without any indication being given as to their nature or their usefulness for the composition or for the cosmetic formulation.
  • the CleanWell patent US6346281 proposes combining citronella essential oil with metal ions, such as copper sulphate, and with a “biosurfactant” and a solvent.
  • the "biosurfactant” can be either "BOD” or Tween-80 which is a polyethoxylated sorbitan.
  • the solvent can be chosen from organic solvents such as ethanol.
  • the combination of thyme oil with copper ions Cu2+ and an alkylpolyglucoside makes it possible to obtain a composition capable of foaming, useful for the treatment and prevention of bacterial infections resistant to antibiotics, in particular methicillin-resistant strains of Staphylococcus aureus.
  • the Reckitt Benckiser patent US5403587 combines an essential oil of thyme or lemongrass with an ethoxylated fatty acid, a “nonoxynol-10” carboxylic acid, or a coconut fatty acid sodium salt, and with a surfactant and an organic solvent.
  • the surfactant and the organic solvent are essential to provide a composition in liquid form capable of being dispersed or solubilized.
  • the surfactant can be chosen from anionic or amphoteric surfactants. These combinations exhibit antibacterial activity on S. Aureus and on P. Aeruginosa.
  • the Procter & Gamble patent W02008/126057 discloses antimicrobial compositions for the care of the mouth. They include a mixture of essential oils containing acyclic compounds and cyclic compounds. The addition of gluconic acid is recommended for its chelating power of the calcium ions located on the walls of the bacteria, which contributes to improving the bactericidal power of the composition.
  • the composition can include all surfactants, but anionic surfactants, cationic surfactants, or zwitterionic surfactants are preferred.
  • Nonionic surfactants are also cited, and the patent emphasizes nonionic surfactants prepared by condensation of alkylene oxide, i.e. polyethoxylated nonionic surfactants.
  • Indusco US9687002 proposes putting lemongrass essential oil in a microemulsion in water with citric acid, lactic acid or acetic acid added as a pH buffer.
  • the microemulsion is obtained thanks to at least two surfactants having an HLB between 9 and 18, and these surfactants can be nonionic surfactants.
  • the microemulsion makes it possible to obtain a stable composition, i.e. remaining macroscopically homogeneous, and transparent.
  • L'Oreal FR3061010 discloses essential oil nanoemulsions obtained by emulsification of these essential oils in a mixture of water and water-soluble organic solvent with surfactants chosen from anionic, nonionic, amphoteric, zwitterionic or cationic surfactants. These nanoemulsions are prepared for their topical use for the treatment of bacterial or fungal infections. Lemongrass essential oil is presented although no antimicrobial activity is attributed to it.
  • nonionic surfactants alkyl polyglucosides are preferred, and particularly caprylyl/capryl glucoside, such as OramixTM CG110 from Seppic.
  • OramixTM CG110 is formulated with ten essential oils, ethanol and water.
  • the amount of OramixTM CG110 used therein is 0.05% by weight relative to the total weight of the formulation.
  • L'Oréal FR3061010 recommends using an amount of nonionic surfactant of less than 1% by weight relative to the total weight of the nanoemulsion. It is the combination of a nonionic surfactant and ethanol which makes it possible to obtain a nanoemulsion. This state of nanoemulsion has advantages in terms of texture, softness to the touch, and transparency.
  • essential oils are natural extracts insoluble in water, known since antiquity for their antiseptic activities, but also for their potential allergenicity, which requires finding, for their use in cosmetics, a dose balanced between the need to increase this dose, to increase the antiseptic activity, and the need to reduce this dose, so as not to cause an allergy.
  • the antiseptic activity has the widest possible spectrum, in order to be able to inhibit the growth or kill all microorganisms, namely bacteria, fungi, yeasts, and viruses.
  • composition of a cosmetic product is very different from that of an in-vitro test culture medium.
  • interactions between the constituents of the antimicrobial composition and the ingredients of the cosmetic product may occur, resulting in the alteration or suppression of the antimicrobial activity. It may then be necessary to increase the dose of antimicrobial composition to regain the antimicrobial activity in situ.
  • a preservative activator composed of natural products or products of natural origin, biodegradable, devoid of ethoxylated or silicone compounds, transparent and which can be integrated into a cosmetic product without altering the physical properties -chemicals of the product, that is to say without altering or destabilizing the cosmetic product, or causing a phase shift or the formation of solid particles, and this for the majority of dosage forms. It is also necessary to develop a formulation that preserves the antimicrobial properties of the activator.
  • FIG. 1 shows the results of antimicrobial activity testing of the antimicrobial liquid composition on Escherichia coli ATCC® 8739.
  • Fig. 2 [0021][Fig. 2] shows the results of antimicrobial activity testing of the antimicrobial liquid composition against Candida albicans ATCC® 10231.
  • FIG. 3 shows the results of antimicrobial activity testing of the antimicrobial liquid composition against Aspergillus brasiliensis ATCC® 16404.
  • FIG. 4 shows the results of antimicrobial activity testing of the antimicrobial liquid composition against Staphylococcus aureus ATCC® 6538.
  • FIG. 5 shows the results of antimicrobial activity testing of the antimicrobial liquid composition against Pseudomonas aeruginosa ATCC® 9027.
  • antimicrobial compositions according to the invention make it possible to activate preservatives and increase their antimicrobial protection.
  • strong logarithmic reductions in the number of colony-forming units of Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans and Staphylococcus Aureus are measured when the antimicrobial compositions are introduced into the cosmetic composition, in combination with a preservative, and this compared to a cosmetic composition comprising only a preservative usually used.
  • the present invention relates to the use of an antimicrobial liquid composition for activating the preservatives of cosmetic products, said antimicrobial liquid composition comprising:
  • At least one essential oil chosen from the essential oils of species of the genus Cymbopogon, the essential oils of clove, Bourbon geranium, noble laurel, lemony litsea, lemon balm, pepper, crown pepper, oregano, tea tree, thyme, lemongrass;
  • At least one nonionic surfactant chosen from alkyl(poly)glycosides, alkylglycosides, esters of vegetable oils, non-ethoxylated fatty esters of polyols, heteropolymers of C8-C10 alkylglycosides and sorbitan fatty esters, or mixtures thereof,
  • At least one carboxylic acid in free form At least one carboxylic acid in free form.
  • the present invention also relates to antimicrobial compositions comprising
  • compositions advantageously make it possible to stabilize the cosmetic products in which they are incorporated, without altering or destabilizing the cosmetic product, or causing a phase shift or the formation of solid particles.
  • the antimicrobial compositions according to the invention keep their antimicrobial activity once formulated in a cosmetic product.
  • the present invention also relates to cosmetic products comprising antimicrobial compositions according to the invention and at least one preservative.
  • the constituents other than water of the antimicrobial composition that is the subject of the present application are sometimes marketed in the form of aqueous solutions, composed of water and one of said constituents.
  • the mass percentages of said constituents other than water in the antimicrobial composition expressed in% by dry weight, are the mass percentages of the dry masses into said constituents, in other words the mass percentages of said dry constituents, water being excluded.
  • the liquid antimicrobial composition which is the subject of the present application is an aqueous composition.
  • the quantities of liquid antimicrobial composition used are expressed in gross mass percentages, denoted as % by gross weight, accounting for the antimicrobial liquid composition in its entirety, in other words taking into account all of its constituents, including water.
  • the present invention relates to the use of an antimicrobial liquid composition for activating the preservatives of cosmetic products, said antimicrobial liquid composition comprising:
  • At least one essential oil chosen from the essential oils of species of the genus Cymbopogon, the essential oils of clove, Bourbon geranium, noble laurel, lemony litsea, lemon balm, pepper, crown pepper, oregano, tea tree, thyme, lemongrass or a mixture of these oils;
  • At least one non-ionic surfactant chosen from alkyl (poly) glycosides, alkyl glycosides, alkyl glycosides, esters of vegetable oils, non-ethoxylated fatty esters of polyols, heteropolymers of C8-C10 alkylglycosides and sorbitan fatty esters, or mixtures thereof,
  • the present invention relates to the use of an antimicrobial liquid composition to activate the preservatives of cosmetic products, said antimicrobial liquid composition comprising:
  • At least one essential oil chosen from the essential oils of species of the genus Cymbopogon, the essential oils of clove, Bourbon geranium, noble laurel, lemony litsea, lemon balm, pepper, crown pepper, oregano, tea tree, thyme, lemongrass or a mixture of these oils;
  • At least one nonionic surfactant chosen from alkyl(poly)glycosides,
  • an antimicrobial composition is a composition which exhibits antimicrobial activity, that is to say that the composition is capable of slowing down the growth of at least certain bacteria, fungi or yeasts, better at inhibiting the growth and lowering the presence in number of at least some of them by preventing them from developing and multiplying, and even better at make their presence undetectable and make them completely disappear by killing them. Therefore, the definition encompasses growth retardation, growth inhibition under the known terms bacteriostatic and fungistatic, and also lethal activity, known as bactericidal or fungicidal.
  • the antimicrobial composition according to the invention proves by itself insufficiently effective in preserving a cosmetic product (i.e. it does not significantly slow down or inhibit the growth of bacteria or fungi and does not have bactericidal or fungicidal activity).
  • the antimicrobial composition according to the invention combines its antimicrobial activity with the activity of said preservative, and potentiates the activity of said preservative. It will then be possible to use a reduced dose of preservative, in combination with an appropriate dose of antimicrobial composition, to successfully reduce the load of microorganisms in the cosmetic product, that is to say reduce the number of colony-forming unit, or even preferentially to stabilize the microbiology of the cosmetic product according to the ISO 11930:2019 standard.
  • the antimicrobial composition thus effectively makes it possible to reduce the quantity of preservative necessary to preserve the cosmetic product, and this over periods equivalent to the usual preservatives used at the recommended doses, which are generally equal to the maximum concentrations permitted in ready-to-use cosmetic products.
  • Preservatives in cosmetic products are present in the cosmetic composition, either alone or in combination, in a content of approximately 1% by weight, relative to the total weight of the composition.
  • the antimicrobial compositions according to the invention make it possible to reduce the preservative content (for example 0.4% for potassium sorbate and sodium benzoate), and to use only one preservative.
  • a preservative activator is a compound which has insufficient antimicrobial activity by itself in the cosmetic product, but which is capable of increasing the antimicrobial activity of a preservative in the cosmetic product.
  • the term “insufficient antimicrobial activity” means a compound which does not make it possible, in a significant manner, to slow down the growth of bacteria, fungi or yeasts, and even less to inhibit their growth or kill them.
  • the preservative activator cannot therefore microbiologically stabilize a medium by itself, and therefore cannot be qualified as a preservative within the meaning of the regulations.
  • a preservative with a preservative activator therefore makes it possible to at least increase the antimicrobial activity of the preservative and preferably to stabilize a cosmetic product microbiologically. It is generally desired that this stabilization or increase occur at a dose of preservative lower than the dose required when the preservative is used alone.
  • the antimicrobial activity can be evaluated by any method known to those skilled in the art.
  • the classification can be made by monitoring the reduction in the number of colony-forming units (denoted cfu/mL) at seven, fourteen and twenty-eight days after the cosmetic product has been inoculated with a microorganism.
  • the reduction in the number of colony forming units is expressed in logarithm base 10, for example one log of reduction corresponds to a reduction of 10 A 1 , i.e. 10, cfu/mL, or two logs of reduction correspond to a reduction of 10 At 2, i.e. 100, cfu/mL.
  • the antimicrobial activity is evaluated according to the international standard ISO 11930:2019 entitled "ISO11930 Cosmetics - Microbiology - Evaluation of the antimicrobial protection of a cosmetic product” which specifies a procedure for the interpretation of the data resulting from the test of the effectiveness of the antimicrobial protection and/or the assessment of the microbiological risk during the overall evaluation of the antimicrobial protection of a cosmetic product.
  • a composition will be considered as a preservative activator when, combined with the preservative, it makes it possible to increase by at least 1 log the reduction in the number of colony-forming units of microorganisms present in the medium, preferably at least two logs, preferably at least 3 logs, compared to the number of colony forming units when the preservative alone is used.
  • a composition will be considered as a preservative activator when combined with the preservative, it makes it possible to increase by at least 1 log the reduction in the number of units forming colonies of microorganisms present in the medium, preferentially to the at least two logs, preferably at least 3 logs, compared to the number of colony-forming units of microorganisms when the preservative alone is used, over a period of at least 7 days, preferably 14 days and even more preferably over a period of at least 28 days.
  • the antimicrobial liquid composition that is the subject of the present application can be qualified as a liquid composition with a preservative-activating effect because it satisfies the preceding definition of preservative-activating agent.
  • the antimicrobial liquid composition is therefore a liquid composition with a preservative-activating effect.
  • the antimicrobial composition according to the invention makes it possible to activate a preservative and, combined with said preservative, to reduce by at least one log, preferably at least two logs, preferably at least three logs, the number of colony forming units of Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans and Staphylococcus aureus.
  • the antimicrobial composition according to the invention makes it possible to activate a preservative and, combined with said preservative, to reduce by at least one log, preferentially by at least two logs, preferentially by at least 3 logs, the number of colony-forming units of Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans and Staphylococcus aureus, over a period of at least 7 days, preferably at least 14 days and preferably at least 28 days.
  • the antimicrobial composition comprises an essential oil chosen from essential oils of species of the genus Cymbopogon, essential oils of clove, Bourbon geranium, noble laurel, lemon-litsea, lemon balm , chili, crown pepper, oregano, tea tree, thyme, lemongrass or a mixture of these oils.
  • the essential oil is chosen from essential oils of species of the genus Cymbopogon.
  • Cymbopogon is a genus of monocotyledonous plants of the Poaceae family, Panicoideae subfamily, which comprises about fifty species originating from the tropical and subtropical regions of Africa, Asia and Australia. They are herbaceous plants, generally perennial, rarely annual, cespitose or rhizomatous, whose stems (culms) can reach 15 to 300 cm in length.
  • the essential oil of species of the genus Cymbopogon is chosen from oils of species of the genus Cymbopogon rich in citral, neral, geranial and geraniol.
  • the essential oil of species of the genus Cymbopogon is chosen from essential oils of species of the genus Cymbopogon having approximately 30% by weight in neral, approximately 40% by weight in geranial, and 5% by weight in geraniol. These mass percentages are usually determined by chromatography.
  • Cymbopogon nardus also called Ceylon lemongrass or Sri Lankan lemongrass
  • Cymbopogon schoenanthus also called Camel grass or geranium grass
  • Cymbopogon winterianus Jowitt also called Java Lemongrass - Cymbopogon martinii var. sofia, also called gingergrass
  • the Cymbopogon essential oil is chosen from the essential oils of the Cymbopogon flexuosus Stapf species. and Cymbopogon citratus (DC.) Stapf.
  • the essential oil is an essential oil of citronella of the species Cymbopogon citratus (DC.) Stapf.
  • essential oils of Cymbopogon flexuosus Stapf. and Cymbopogon citratus (DC.) Stapf. have about 30% by weight neral, about 40% by weight geranial, and 5% by weight geraniol
  • the essential oil can also be advantageously chosen from other oils rich in citral, neral, geranial and geraniol.
  • It may be, for example, essential oil of lemon bedsea which contains approximately 40% by weight of geranial and approximately 30% by weight of neral or essential oil of lemon balm of the species Melissa officinalis, compared to the total weight of essential oil.
  • an essential oil rich in geraniol and geraniol such as in particular the essential oil of palmarosa (Cymbopogon martini) which usually contains between 80% and 85% by weight of geraniol relative to the total weight of essential oil.
  • the essential oil will comprise at least one active molecule chosen from the active molecules that make up the essential oil lemongrass of the species Cymbopogon flexuosus and Cymbopogon citratus: the trans isomer of citral, known as geranial or citral A, with the name IIICPA (E)-3,7-Dimethylocta-2,6-dienal; the cis isomer of citral, known as neral, or citral B, of the name IIICPA (Z)-3,7-Dimethylocta-2,6-dienal; geraniol, named IIICPA (2E)-3,7-dimethylocta-2,6-dien-1-ol.
  • the trans isomer of citral known as geranial or citral A, with the name IIICPA (E)-3,7-Dimethylocta-2,6-dienal
  • the cis isomer of citral known as neral, or citral B, of the
  • the essential oil is chosen from the essential oils of Cymbopogon, lemon-litsea, lemon balm.
  • the essential oil useful for the antimicrobial composition that is the subject of the present application can be chosen from the essential oils of ajwain (also called Indian thyme), star anise (also called star anise ), basil, Chinese or Ceylon cinnamon, cardamom, cypress from governing, lemon eucalyptus, eucalyptus globulus, eucalyptus radiata, black spruce, tarragon, fennel, wintergreen , Virginia juniper, grass geranium, rose geranium, Bourbon geranium, gingergrass, clove (clove), fragrant inula, noble laurel, reydovan lavandin, fine lavender, cineole aspic lavender, true lavender, lavandin, super lavandin, garden marjoram, shell marjoram, linear-leaved tea tree, field mint, peppermint, lemon balm, red myrtle, neroli, niaouli, petit grain big
  • the essential oil may also be an oil rich in phenols, in particular in carvacrol (present for example in the essential oil of savory), in thymol (present for example in the essential oil of thyme with thymol) and in eugenol (present for example in clove essential oil). These phenols are responsible for the fungicidal and bactericidal activities of the essential oils that contain them.
  • Mention may more particularly be made, as oils rich in phenols, of the essential oils of thyme (Thymus mastichina, Thymus vulgaris, Thymus zygis, Thymus thymi), pepper (Pimenta racemosa, Pimenta acris), ajowan (Trachyspermum ammi), clove (Eugenia caryophyllus), mountain savory (Satureja montana), oregano (Origanum heracleoticum (Greek oregano), Origanum majorana, Origanum vulgare, Origanum compactum (Oregano compact), Spanish oregano (Corydothymus capitatus), Ceylon cinnamon (Cinnamomum verum).
  • the essential oil will comprise at least one active molecule chosen from monoterpenols, which are alcohols with 10 carbon atoms, preferably geraniol, linalool, thujanol, myrcenol, terpineol, menthol and piperitol.
  • Essential oils that include these active molecules are palmarosa Cymbopogon martinii, spike lavender Lavandula spica, peppermint Mentha piperita, marjoram Origanum majorana, and tea tree essential oils. species Melaleuca alternifolia.
  • another essential oil poor in at least one phenol, monoterpenol, terpene oxide, aromatic aldehyde, terpene aldehyde, phenylpropene, monoterpene hydrocarbon, and sesquiterpene hydrocarbon can be added to the composition object of the present application, for example to perfume it, change its smell or act on its antimicrobial activity. It can be chosen from essential oil of cedar, essential oil of sweet orange, essential oil of lemon, essential oil of green or red mandarin, or essential oil of wintergreen.
  • the total quantity of essential oils present in the antimicrobial liquid composition can range from 0.1% to 10% by dry weight, preferentially from 0.5% to 7% by dry weight, more preferentially from 1% to 5 % by dry weight, and most preferably from 1.5% to 3% by dry weight, relative to the total weight of the antimicrobial liquid composition.
  • the ratio of the total dry mass of nonionic surfactants to the total dry mass of essential oils may also be greater than or equal to 2, preferably greater than or equal to 3, more preferably greater than or equal to 4, and any preferably greater than or equal to 5.
  • the essential oil(s) are advantageously present in the antimicrobial composition in a quantity which is lacking with respect to the quantity of nonionic surfactant(s). The selection of this default situation makes it possible to best solubilize the essential oil or oils in the water of the antimicrobial liquid composition, and also contributes to maintaining this solubilization in the water of the cosmetic product when the said liquid composition antimicrobial is diluted in said cosmetic product, and in particular in the water of said cosmetic product.
  • This ratio advantageously makes it possible to obtain a stable antimicrobial liquid composition, without phase shift or precipitation over time, while being transparent or opalescent, in the concentrated state or even after high dilution in water.
  • the nonionic surfactant is chosen from:
  • alpha-diols and (C1-C20)alkylphenols these compounds being polyethoxylated and/or polypropoxylated and/or polyglycerolated, the number of ethylene oxide and/or propylene oxide groups possibly ranging from 1 to 100, and the number of glycerol groups possibly ranging from 2 to 30; or alternatively these compounds comprising at least one fatty chain comprising from 8 to 40 carbon atoms, in particular from 16 to 30 carbon atoms; in particular alcohols comprising at least one C8 to C40 alkyl chain, saturated or not, linear or branched, oxyethylenated comprising from 1 to 100 moles of ethylene oxide, preferably from 2 to 50, more particularly from 2 to 40 moles of ethylene oxide and comprising one or two fatty chains;
  • polyethoxylated fatty amides preferably having from 2 to 30 ethylene oxide units, polyglycerolated fatty amides comprising on average from 1 to 5 glycerol groups and in particular from 1.5 to 4;
  • polyoxyalkylenated fatty acid esters preferably polyoxyethylenated, having from 2 to 150 moles of ethylene oxide, including oxyethylenated vegetable oils;
  • amine oxides such as (C10-C14 alkyl)amine oxides or N-(C10-C14 acyl)-aminopropylmorpholine oxides; - non-ethoxylated fatty esters of polyols, and in particular from non-ethoxylated fatty esters of glycerol, polyglycerols, sorbitol, sorbitan, androdrohexitols such as in particular isosorbide, mannitol, xylitol, erythritol, maltitol, sucrose, glucose, polydextrose, hydrogenated glucose syrups, dextrins and hydrolyzed starches,
  • esters of polyglycerol and saturated or unsaturated C4-C20 fatty acids preferably C8-C18, and more preferably C18, for example polyglyceryl-2 dipolyhydroxystearate and polyglyceryl-3 diisostearate,
  • - vegetable oil esters in particular from coconut oil esters, for example coco-caprylate, and mixtures thereof.
  • the nonionic surfactant is chosen from alkyl(poly)glycosides, which are represented by the following general formula:
  • Ri represents: a linear or branched alkyl or alkenyl radical containing 6 to 24 carbon atoms, or 6 to 18 carbon atoms, or 6 to 12 carbon atoms; or an alkylphenyl radical whose linear or branched alkyl radical contains 6 to 24 carbon atoms, or 6 to 18 carbon atoms, or 6 to 12 carbon atoms,
  • R 2 represents an alkylene radical containing 2 to 4 carbon atoms
  • - G represents a sugar unit comprising 5 to 6 carbon atoms
  • - 1 denotes a value ranging from 0 to 10, preferably from 0 to 4,
  • - v denotes a value ranging from 1 to 15, preferably from 1 to 4.
  • alkyl(poly)glycoside surfactants are compounds of the formula described above in which:
  • Ri denotes a saturated or unsaturated, linear or branched alkyl radical comprising from 6 to 18 carbon atoms, or from 6 to 12 carbon atoms,
  • R 2 represents an alkylene radical containing 2 to 4 carbon atoms
  • - 1 denotes a value ranging from 0 to 3, preferably equal to 0,
  • G denotes glucose, fructose or galactose, preferably glucose
  • the degree of polymerization that is to say the value of v, which can range from 1 to 15, preferably from 1 to 4; the average degree of polymerization being more particularly between 1 and 2.
  • the glucosidic bonds between the sugar units are generally of the 1-6 or 1-4 type, preferably of the 1-4 type.
  • the alkyl(poly)glycoside surfactant is an alkyl(poly)glucoside surfactant, that is to say an alkyl(poly)glycoside surfactant where G is glucose.
  • G is glucose.
  • the surfactant is chosen from capryl/capryl glucosides.
  • the nonionic surfactant can also be chosen from alkyl(poly)glycosides, preferably alkyl(poly)glucosides, with an HLB greater than or equal to 10, or greater than or equal to 12, or greater than or equal to 14.
  • Alkyl(poly)glycosides preferably alkyl(poly)glucosides, can also be combined with fatty alcohols.
  • the nonionic surfactant can also be chosen from heteropolymers of C8-C10 alkylglycosides and fatty esters of sorbitan, preferably from heteropolymers of C8-C10 alkylglycosides and C4-C20 fatty esters of sorbitan, and more preferably from heteropolymers of C10 alkylglycosides and of C18 fatty esters of sorbitan.
  • An example of such a heteropolymer is Poly Suga® Mulse D9 from Colonial Chemical Inc.
  • the total amount of nonionic surfactants in the antimicrobial liquid composition is greater than or equal to 1% by weight, preferably greater than or equal to 5% by weight, more preferably greater than or equal to 7.5% by weight, and any preferably greater than or equal to 10% by weight, relative to the total weight of said liquid antimicrobial composition.
  • the total quantity of nonionic surfactants present in the liquid antimicrobial composition can range from 1% to 50% by weight, preferentially from 1% to 40%, preferentially from 5% to 40% by weight, preferentially 5% to 30% by weight, more preferably from 7.5% to 30% by weight, more preferably 7.5 to 20% by weight, and most preferably from 10% to 20% by weight, relative to the total weight of the composition antimicrobial liquid.
  • the ratio of the total dry mass of nonionic surfactants to the total dry mass of essential oils may also be greater than or equal to 2, preferably greater than or equal to 3, more preferably greater than or equal to 4, and any preferably greater than or equal to 5.
  • the nonionic surfactant(s) are advantageously present in the antimicrobial composition in an amount which is in excess relative to the amount of the essential oil(s). The selection of this excess situation makes it possible to best solubilize the essential oil or oils in the water of the antimicrobial liquid composition, and also contributes to maintaining this solubilization in the water of the cosmetic product when the said antimicrobial liquid composition is diluted in said cosmetic product, and in particular in the water of said cosmetic product.
  • a value of the ratio of the mass of caprylyl/capryl glucoside to the mass of essential oil greater than or equal to 2, preferably greater than or equal to 3, more preferably greater than or equal to 4, most preferably greater than or equal to 5, makes it possible to obtain a completely transparent and stable antimicrobial liquid composition over time in the concentrated state and in the diluted state in the water.
  • Cosmetic product formulators generally prefer to employ transparent ingredients to formulate their products.
  • the selection of nonionic surfactants according to the invention makes the liquid antimicrobial composition compatible with ionic surfactants and zwitterionic surfactants. It is therefore possible to add the composition antimicrobial to a cosmetic product comprising another type of surfactant while maintaining good physical stability of the state of the cosmetic product, and retaining the effects of ionic or zwitterionic surfactants, that is to say without masking or neutralizing the effects of these surfactants.
  • the antimicrobial composition according to the invention can be added to shampoos or shower gels, which comprise anionic surfactants, often in high quantities, while retaining the detergent power of the anionic surfactants, and retaining the monophasic state liquid or gel.
  • the liquid antimicrobial composition can also be added to a coloring solution or hair conditioner, generally comprising cationic surfactants or cationic polymers, while retaining the coloring ability and conditioning ability of the hair.
  • the free carboxylic acid useful for the antimicrobial composition which is the subject of the present application is chosen from monocarboxylic acids and polycarboxylic acids, linear or branched, preferentially from monocarboxylic acids, dicarboxylic acids, and tricarboxylic acids, very preferentially among monocarboxylic acids and dicarboxylic acids.
  • free it is meant that the carboxylic acid function is either in its protonated form COOH, or in its ionized form COO- associated with a counter ion H+ or H3O+, and this in proportions dependent on the value of the pH. of the aqueous solution of acid and the strength of the acid characterized by its pKa.
  • the carboxylic acid is chosen from monocarboxylic acids whose carbon chain consists of 2 to 12 carbon atoms, or 3 to 8 carbon atoms.
  • monocarboxylic acids whose carbon chain consists of 2 to 12 carbon atoms, or 3 to 8 carbon atoms.
  • lactic acid glycolic acid
  • glucuronic acid maltobionic acid
  • lactobionic acid malic acid
  • tartaric acid mandelic acid
  • fatty acids (or aliphatic chain carboxylic acids) having a carbon chain of 4 to 12 atoms preferably natural fatty acids such as in particular propionic, butyric, caproic, caprylic, capric and lauric acids.
  • the carboxylic acid is chosen from gluconic acid, glucuronic acid, maltobionic acid, preferentially the carboxylic acid is gluconic acid.
  • the monocarboxylic acid is the cyclic form of gluconic acid, called gluconolactone.
  • the carboxylic acid is chosen from polycarboxylic acids, and preferably from dicarboxylic acids and tricarboxylic acids, and most preferably from aspartic acid, adipic acid, malonic, pimelic acid, succinic acid, glucaric acid, and glutaric acid, and even more preferably is succinic acid.
  • carboxylic acid(s) or polycarboxylic acid(s) useful for the antimicrobial liquid composition which is the subject of the present application are further characterized by a pKa value ranging from 3 to 6, preferably from 4 to 6.
  • the total amount of free carboxylic acid(s) present in the liquid antimicrobial composition can range from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight. dry weight, and most preferably from 27.5% to 40% by dry weight, relative to the total weight of the antimicrobial liquid composition.
  • the carboxylic acid salt useful for the antimicrobial composition which is the subject of the present application is chosen from salts of monocarboxylic acids or salts of linear or branched polycarboxylic acids.
  • the carboxylic acid function is either in the protonated form COOH, or in the ionized form COO- associated with a metallic counter ion M+, and this in proportions dependent on the pH value of the aqueous acid solution , the acidity constant pKa of the corresponding free acid, and the dissociation constant of the salt pKd.
  • the carboxylic acid salt or salts is or are chosen from sodium, magnesium, zinc, calcium, potassium, iron, lithium, carboxylic acid salts chosen from the carboxylic acids of "free carboxylic acid" part of the present application.
  • the carboxylic acid salt is a salt of the free carboxylic acid useful for the composition that is the subject of the present application.
  • said carboxylic acid is distributed in at most 35% by dry weight in salt of said carboxylic acid and in at least 65% by dry weight in said free carboxylic acid.
  • gluconic acid distributed at 35% by dry weight as sodium gluconate and 65% by dry weight as free gluconic acid.
  • such a mixture of acid and its salt has a pH that is better tolerated by the skin and is less irritating than the acid alone can be.
  • the carboxylic acid salt or salts is or are chosen from sodium, magnesium, zinc, calcium, potassium, iron or lithium salts of gluconic acid or succinic acid, and preferably the carboxylic acid salt or salts are chosen from sodium gluconate and sodium succinate, and most preferably the carboxylic acid salt is sodium gluconate.
  • the total quantity of carboxylic acid salts present in the liquid antimicrobial composition can range from 1% to 50% by dry weight, preferentially from 5% to 30% by dry weight, more preferentially from 10% to 20% by dry weight. dry weight, and most preferably from 15% to 17.5% by dry weight, relative to the total weight of the antimicrobial liquid composition.
  • the water present in the antimicrobial liquid composition can be decarbonated water, or demineralized water.
  • the amount of water present in the antimicrobial liquid composition can range from 20% to 75% by weight, preferably from 30% to 65% by weight, more preferably from 35% to 55% by weight, relative to the weight total antimicrobial liquid composition.
  • the pH of the antimicrobial liquid composition that is the subject of the present application can range from 2 to 9, preferably from 3 to 8, more preferably from 4 to 7, and even more preferably from 4.5 to 6.5, and even more more preferably from 5.5 to 6.2.
  • the preservative can be chosen from propionic acid, calcium propionate, formaldehyde, paraformaldehyde, o-phenylphenol or its salts, zinc pyrithione, sodium sulphites, bisulphites or metabisulphites, d ammonium, potassium, chlorobutanol, methylparaben, ethylparaben, propylparaben, butylparaben, formic acid and its salts such as sodium formate, benzoic acid and its salts such as sodium benzoate, sorbic acid and its salts, such as calcium sorbate, sodium sorbate, potassium sorbate, salicylic acid and its salts, dehydroacetic acid and its salts such as sodium dehydroacetate, undecylenic acid and its salts such as calcium undecylenate, potassium undecylenate, sodium undecylenate, phenoxyethanol, 1,2-dimethylol-5,6-dimethylhydantoin,
  • the antimicrobial composition is a preservative activator for the following preservatives: benzoic acid, sodium benzoate, salicylic acid and its salts, sorbic acid, calcium sorbate, sodium sorbate, potassium sorbate, dehydroacetic acid, sodium dehydroacetate, undecylenic acid, calcium undecylenate, potassium undecylenate, sodium undecylenate, phenoxyethanol, 1,2-Dimethylol-5,6-dimethylhydantoin, benzyl alcohol, chlorhexidine, chlorhexidine diacetate, chlorhexidine digluconate, dihydrochloride chlorhexidine, behentrimonium chloride, cetrimonium chloride, cetrimonium bromide, laurtrimonium chloride, laurtrimonium bromide, steartrimonium chloride, steartrimonium bromide, hexamidine, hexamidine diisethionate, chlorphenesin
  • the preservative is chosen from formic acid and its salts, dehydroacetic acid and its salts, benzoic acid and its salts, sorbic acid and its salts, phenoxyethanol, benzyl alcohol and its salts. More preferably, the preservative activated by the liquid antimicrobial composition is chosen from benzoic acid, sorbic acid, phenoxyethanol, benzyl alcohol, sodium benzoate, potassium sorbate. Even more preferably, the preservative is chosen from phenoxyethanol, benzyl alcohol, sodium benzoate and potassium sorbate.
  • the preservative activated by the liquid antimicrobial composition is chosen from sorbic acid and its calcium, sodium, potassium, magnesium or zinc salts, or a mixture of these. this. Even more preferably, the preservative is chosen from sorbic acid, calcium sorbate, sodium sorbate, potassium sorbate. Most preferably, the preservative is potassium sorbate.
  • the antimicrobial composition according to the invention makes it possible to activate the preservative power of phenoxyethanol against Pseudomonas Aeruginosa, Escherichia Coli, Staphylococcus aureus and Aspergillus brasiliensis.
  • the antimicrobial composition according to the invention makes it possible to activate phenoxyethanol and, combined with said phenoxyethanol, to reduce by at least two logs the number of colony-forming units of Pseudomonas Aeruginosa, Staphylococcus aureus , Aspergillus brasiliensis and Escherichia Coli.
  • the antimicrobial composition according to the invention makes it possible to activate phenoxyethanol and thus allows a reduction in the number of colony-forming units compared to phenoxyethanol alone, greater:
  • the antimicrobial composition according to the invention makes it possible to activate the preservative power of benzyl alcohol against Pseudomonas Aeruginosa, Staphylococcus aureus, and Escherichia Coli.
  • the antimicrobial composition according to the invention makes it possible to activate benzyl alcohol and thus allows a reduction in the number of colony-forming units compared to benzyl alcohol alone, greater:
  • the antimicrobial composition according to the invention makes it possible to activate the preservative power of sodium benzoate against Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis, and Candida albicans.
  • the antimicrobial composition according to the invention makes it possible to activate sodium benzoate and thus allows a reduction in the number of colony-forming units compared to sodium benzoate alone, greater than:
  • the antimicrobial composition according to the invention makes it possible to activate the preservative power of potassium sorbate against Pseudomonas Aeruginosa, Staphylococcus aureus, Escherichia Coli, Candida Albicans and 'Aspergillus brasiliensis.
  • the antimicrobial composition according to the invention makes it possible to activate potassium sorbate and thus makes it possible to reduce the number of colony-forming units compared to potassium sorbate alone, greater than:
  • an antimicrobial liquid composition to activate a cosmetic product preservative in a cosmetic product can be made with:
  • an amount of antimicrobial liquid composition which can range from at least 0.1% by gross weight, preferably at least 0.5% by gross weight, more preferably at least 0.75% by gross weight, preferably at least 1 % by gross weight, and even more preferably at least 1.5% by gross weight,
  • preservative which can be up to 2.5% by gross weight, preferably up to 1.5% by gross weight, more preferably up to 1% by gross weight, preferably up to 0 7% by gross weight, and even more preferably up to 0.6% by gross weight, relative to the total weight of the cosmetic product.
  • an antimicrobial liquid composition to activate a cosmetic product preservative in a cosmetic product can be made with:
  • an amount of antimicrobial liquid composition which can range from 0.1% to 5% by gross weight, preferably from 0.5% to 3% by gross weight, more preferably from 0.75% to 2% by gross weight, and most preferably from 1% to 1.5% by gross weight, of said at least one antimicrobial liquid composition,
  • an amount of usual preservative which can be from 0.1% to 2.5% by gross weight, preferably from 0.2% to 1.5% by gross weight, more preferably from 0.3% to 1 % by gross weight, and most preferably from 0.4% to 0.7% by gross weight, relative to the total weight of the cosmetic product.
  • the antimicrobial composition makes it possible to reduce by at least 35%, or even by at least 50%, or even better still by at least 60%, the quantity of usual preservative used in the cosmetic formulations. Thus it is generally possible to use them only at very low levels not exceeding 0.5% by gross weight, or even 0.4% by gross weight, relative to the total weight of the cosmetic product.
  • the microbiological stability may be equal or even better than with the usual preservative used alone and at the recommended dose.
  • the antimicrobial composition that is the subject of the present application comprises, or consists of:
  • an essential oil consisting of citral and geraniol preferably a lemongrass oil consisting of citral and geraniol
  • alkylglucoside carrying fatty chains with 6 to 12 carbon atoms preferably caprylyl/capryl glucoside
  • carboxylic acid salt preferably sodium gluconate or sodium succinate, most preferably sodium gluconate
  • the antimicrobial composition comprises, or consists of:
  • an essential oil preferably lemongrass comprising at least 50% by weight of citral and geraniol relative to the weight of said essential oil, at a mass percentage of 0.1% to 10% by dry weight, preferably 0, 5% to 7% by dry weight, more preferably from 1% to 5% by dry weight, and most preferably from 1.5% to 3% by dry weight,
  • alkylglucoside carrying fatty chains containing 6 to 12 carbon atoms preferably caprylyl/capryl glucoside, preferably from 5% to 30% by dry weight, more preferably 7, 5% to 20% by dry weight,
  • gluconic acid from 10% to 70% by dry weight of gluconic acid, succinic acid, sodium gluconate or sodium succinate, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
  • the embodiments with terpene aldehydes, and without benzene aldehydes, have the advantage of being generally considered to be less irritating and less allergenic for the skin than the embodiments with benzene aldehydes.
  • the present invention relates to an antimicrobial liquid composition
  • an antimicrobial liquid composition comprising, preferably consisting of:
  • an essential oil chosen from the essential oils of clove, lemongrass, Bourbon geranium, geranium grass, gingergrass, noble laurel, lemongrass, West Indian lemongrass, Indian lemongrass, East Indian, Lemon Bed, Lemon Balm, Palmarose, Chilli, Crown Pepper, Oregano, Tea Tree, Thyme, Lemongrass,
  • nonionic surfactant chosen from alkyl(poly)glycosides, preferably from alkyl(poly)glucosides,
  • the antimicrobial liquid composition comprises, preferably consists of:
  • an essential oil chosen from essential oils of citronella, and essential oils of lemongrass from western India, lemongrass from eastern India, and preferably from essential oils of species of the genus Cymbopogon ,
  • nonionic surfactant chosen from alkyl(poly)glycosides, preferably from alkyl(poly)glucosides,
  • the antimicrobial liquid composition comprises, preferably consists of:
  • the antimicrobial liquid composition comprises
  • - caprylyl/capryl glucoside present at a mass percentage ranging from 1% to 40% by dry weight, preferably from 5% to 30% by dry weight, more preferably from 7.5% to 20% by dry weight,
  • - free gluconic acid present at a mass percentage ranging from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
  • the antimicrobial liquid composition consists of
  • - caprylyl/capryl glucoside present at a mass percentage ranging from 1% to 40% by dry weight, preferably from 5% to 30% by dry weight, and more preferably from 7.5% to 20% by dry weight,
  • - free gluconic acid present at a mass percentage ranging from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
  • an essential oil chosen from the essential oils of clove, lemongrass, Bourbon geranium, geranium grass, gingergrass, noble laurel, lemongrass, West Indian lemongrass, Indian lemongrass, East Indian, Lemon Bed, Lemon Balm, Palmarose, Chilli, Crown Pepper, Oregano, Tea Tree, Thyme, Lemongrass,
  • nonionic surfactant chosen from alkyl(poly)glycosides, preferably from alkyl(poly)glucosides,
  • a salt of said carboxylic acid chosen from calcium, sodium, potassium, calcium, magnesium, zinc salts,
  • the object antimicrobial liquid composition comprises, preferably consists of:
  • an essential oil chosen from essential oils of citronella, and essential oils of lemongrass from western India, lemongrass from eastern India, and preferably from essential oils of species of the genus Cymbopogon ,
  • nonionic surfactant chosen from alkyl(poly)glycosides, preferably from alkyl(poly)glucosides,
  • the object antimicrobial liquid composition comprises, preferably consists of:
  • the antimicrobial liquid composition comprises:
  • - caprylyl/capryl glucoside present at a mass percentage ranging from 1% to 40% by dry weight, preferably from 5% to 30% by dry weight, more preferably from 7.5% to 20% by dry weight,
  • - free gluconic acid present at a mass percentage ranging from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
  • - sodium gluconate present at a mass percentage ranging from 1% to 50% by dry weight, preferably from 5% to 30% by dry weight, more preferably from 10% to 20% by dry weight, and most preferably 15% at 17.5% by dry weight,
  • the antimicrobial liquid composition consists of:
  • - caprylyl/capryl glucoside present at a mass percentage ranging from 1% to 40% by dry weight, preferably from 5% to 30% by dry weight, and more preferably from 7.5% to 20% by dry weight,
  • - free gluconic acid present at a mass percentage ranging from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
  • - sodium gluconate present at a mass percentage ranging from 1% to 50% by dry weight, preferably from 5% to 30% by dry weight, more preferably from 10% to 20% by dry weight, and most preferably 15% at 17.5% by dry weight,
  • the choice of the constituents of the antimicrobial liquid composition which is the subject of the present application also has the advantage of giving it a content index of natural origin, denoted CNO, of 100%, the alkyl(poly)glucosides being obtained only from from plant resources.
  • the antimicrobial composition that is the subject of the present application is in the form of a liquid, which is a dispersion of an oily phase in an aqueous phase.
  • This dispersion can be either an oil-in-water emulsion, or an oil-in-water microemulsion, or an oil-in-water nanoemulsion, or a micellar solution, depending on the nature and the amounts of the constituents of the composition and its process. of production.
  • the antimicrobial composition is an oil-in-water emulsion, and has oil phase droplet sizes ranging from 0.3 micrometers to 10 micrometers.
  • the antimicrobial composition is an oil-in-water microemulsion or an oil-in-water micellar composition, and has droplet sizes ranging from 0.001 micrometers to 0.3 micrometers. Smaller droplet sizes, or microdroplets, or micelles, of the antimicrobial liquid composition make it opalescent or transparent. In addition, they also contribute to improving the stability of the oil in water, and to improving its antimicrobial activity and its effectiveness as a preservative activator.
  • the oily dispersed phase comprises the essential oil; the aqueous phase comprises the carboxylic acid and/or the carboxylic acid salt; and the surfactant is located at the interface between the two phases.
  • the oily phase may include a "non-essential" oil, such as triglycerides, in order to adjust the concentration of essential oil in the oily phase, and also to reduce the potential allergenicity of the essential oil.
  • the oily phase can also include oils such as methyl esters of vegetable oils, or triglycerides of short fatty acids.
  • the oily phase and the aqueous phase can also comprise additives without antimicrobial activity such as rheology agents, soluble dyes, pigments, perfumes, humectants, bulking agents.
  • the oily dispersed phase consists of the essential oil; the aqueous phase consists of water, free carboxylic acid and/or carboxylic acid salt; and the nonionic surfactant is distributed between the two phases.
  • the aqueous phase contains water as the sole and unique solvent, and is therefore free of any other solvent, in particular of any organic solvent.
  • the transparency of the antimicrobial liquid composition and the compatibility with ionic surfactants allow this antimicrobial composition to be added to cosmetic products that are themselves transparent, such as micellar waters or gels, while retaining the transparency.
  • the antimicrobial liquid composition is in the form of a macroscopically homogeneous liquid, which allows easy use during the production of cosmetic products. Handling a liquid requires less personal or collective protective equipment than handling a pulverulent powder. The transfer between container and the precise dosage are also much simpler and more reliable than for a pulverulent powder.
  • the antimicrobial liquid composition can easily be incorporated into a cosmetic product in order to activate the preservative present, without destabilizing the cosmetic product.
  • This composition according to the invention offers good stability and compatibility with cosmetic products, allowing transparency without problem of crystallization or precipitation.
  • the present application also relates to a cosmetic product containing, as a preservative activator, an antimicrobial liquid composition according to the invention, and at least one usual cosmetic product preservative as described above.
  • the cosmetic product comprises:
  • the cosmetic product comprises:
  • the cosmetic product comprises:
  • the cosmetic product comprises a single and single antimicrobial liquid composition according to the present application, and a single and single preservative.
  • the cosmetic product can be in any known form or physical state, namely an oil-in-water emulsion, a water-in-oil emulsion, a suspension, a foam, a true solution, a micellar solution , a hydroalcoholic solution, a paste, a gel, a powder, a tablet, a wipe.
  • the product is in a form chosen from an oil-in-water emulsion, a water-in-oil emulsion, a suspension, a foam, a true solution, a micellar solution, a hydroalcoholic solution, a paste, a freeze.
  • the product is in a form chosen from an oil-in-water emulsion, a water-in-oil emulsion, a suspension, a foam, a true solution, a micellar solution, a paste, a gel.
  • the cosmetic product due to the neutrality of the composition according to the invention and its high compatibility with the vast majority of oils and fatty substances, alcohols, surfactants, emulsifiers, solubilizers, conditioners, film-forming agents, thickeners, gelling agents , neutralizing agents, or even active agents, can be formulated without particular difficulty and in a very broad manner with the ingredients usually selected.
  • the following protocol describes the preparation of an antimicrobial composition consisting of essential oil(s), gluconic acid, sodium gluconate and a solubilizing surfactant.
  • solubilizing surfactant When the solubilizing surfactant is in the form of a powder, it is dissolved in a minimum quantity of water.
  • This aqueous solution of essential oil(s) and solubilizer is added to an aqueous solution of gluconic acid composed of the required quantity of free gluconic acid and sodium gluconate, with gentle stirring (for example 500- 1000 rpm using a Rayneri motor fitted with a propeller) and at ambient temperature (22° C.), until a homogeneous solution is obtained.
  • the antimicrobial composition Used as a preservative activator, can be added to the cosmetic product at the end of preparation, in other words after the latter has been prepared, when the preparation of said cosmetic product includes high-temperature heating steps. temperature 60-80°C for periods exceeding a few minutes.
  • the antimicrobial composition can be added from the first stages of preparation, but it is preferable to add it at the end of the preparation of the cosmetic product.
  • the antimicrobial composition according to the invention can also find non-cosmetic uses and can in particular be suitable for microbiologically stabilizing pharmaceutical, food or industrial compositions such as, for example, liquid detergent compositions, liquid washing compositions, starch adhesives.
  • Another object of the present application is the use of an antimicrobial composition according to the present application for killing microorganisms, or pathogenic microorganisms, or inhibiting the growth of microorganisms or pathogenic microorganisms, on or in a substrate not living or artificial.
  • an antimicrobial composition for killing microorganisms, or pathogenic microorganisms, or inhibiting the growth of microorganisms or pathogenic microorganisms, on or in a substrate not living or artificial.
  • Such an application concerns, for example, the disinfection of surfaces (floors, walls, doors, door handles), disinfection/conservation of industrial liquid products such as aqueous solutions of starches, proteins, or fibers.
  • Example 1 selection of a solubilizing surfactant to achieve the transparency criteria
  • This example presents the selection of a solubilizing surfactant and the ratio of the gross mass of surfactant to the gross mass of essential oil, to obtain a aqueous solution of essential oil of lemongrass Cymbopogon flexuosus which is transparent both in the concentrated state and in the state diluted in water.
  • a solubilizing surfactant will be acceptable if both transparency criteria are met. Only the main surfactants tested which gave results are presented here.
  • the ratio of the gross mass of surfactant to the gross mass of essential oil is denoted “raw TA/HE ratio” below.
  • the protocol for preparing a liquid composition is as follows:
  • a first premix is prepared by dissolving the gluconic acid in the mass of water with gentle stirring at 20-22°C,
  • a second premix is prepared by adding to the mass of essential oil, the required mass of solubilizing surfactant, and stirring to allow the essential oil to be well dispersed and to obtain a homogeneous liquid,
  • the second pre-mixture is then added to the first pre-mixture, and the mixture is maintained under gentle non-shearing agitation for about 20 minutes, to allow time for the pre-mixture of surfactant and essential oil to disperse, and thus the liquid composition to stabilize.
  • the state of the liquid composition prepared is observed with the naked eye in order to evaluate its transparency and its homogeneity, in particular over the entire height of the sample, and in order to search for the possible presence of several phases or solid particles (which would have formed by instantaneous precipitation, or by slower crystallization).
  • This state is denoted by “concentrated liquid composition”.
  • Concentrated liquid composition On half of the volume of liquid composition, these observations are continued during storage at a temperature of 20-22° C. for 1 month.
  • uccess almost imperceptible opalescence; homogeneous and almost perfect transparency to the naked eye; no turbidity visible to the naked eye.
  • the surfactants A, E and F make it possible to provide a concentrated liquid composition which is transparent.
  • Surfactants B, C and G fail to provide a concentrated liquid composition which is transparent, but allow transparency after dilution in water.
  • Surfactant F provides transparency after dilution in water.
  • the surfactants A, B, C, E, F and G may be suitable for the liquid antimicrobial composition which is the subject of the present application.
  • the solubilizing surfactant F that is to say caprylyl/capryl glucoside
  • the solubilizing surfactant F makes it possible to satisfy both the criterion of transparency and homogeneity of the concentrated liquid composition, and the same criterion after dilution in water, and this for values of the crude TA/HE ratio ranging from 8 to 10.
  • the values of the crude TA/HE ratio ranging from 8 to 10 are equivalent to values of a ratio of the dry mass of surfactant to the dry mass of essential oil ranging from 4 to 5 (because this surfactant comprises 50% water and 50% caprylyl/dry capryl glucoside).
  • Example 2 preparations of antimicrobial compositions
  • compositions of the antimicrobial compositions that are the subject of the present application are shown in Table 5.
  • the antimicrobial compositions 40 and 43 are prepared according to the following protocol:
  • the required quantity of essential oil is slowly added to the required quantity of solubilizing surfactant solution, with gentle stirring, for example 500-1000 rpm using a Rayneri motor equipped with a propeller, and at temperature room temperature of 22°C, until a homogeneous solution is obtained.
  • This aqueous solution of essential oil and solubilizer is added to an aqueous solution of gluconic acid and sodium gluconate.
  • the antibacterial and antifungal activities of the compositions prepared in Example 2 are demonstrated through in vitro growth tests on standard culture media for the following microorganisms: Escherichia coli ATCC® 8739, Pseudomonas Aeruginosa ATCC® 9027, Staphylococcus Aureus ATCC® 6538, Candida Albicans ATCC® 10231, and Aspergillus Brasiliensis ATCC® 16404. These tests include comparisons with the constituents of the compositions taken in isolation, and taken in combination of two constituents, in order to identify the synergies of antimicrobial activity on these microorganisms.
  • test tubes are prepared as there are products to be tested, that is to say the antimicrobial composition, the constituents alone, or the combinations of two constituents, as well as a control, with the culture medium adapted to the microorganism: “potato dextrose broth” for Aspergillus Brasiliensis; “Yeast Molds” for Candida Albicans; “tryptone soy broth” for Escherichia Coli; “medium” for Staphylococcus Aureus; and “middle” for Pseudomonas Aeruginosa.
  • a dose of product to be tested according to Table 6 below, expressed as a weight/volume percentage is then added to each test tube. For example, a percentage of 1.5% weight/volume means that for 100 mL of culture medium, 1.5 g of product to be tested are added. Then we homogenize carefully by suction-repression.
  • Each test tube is inoculated with a known quantity of microorganisms : 10 to 3 colony-forming units per milliliter of agar (denoted cfu/mL) for Aspergillus brasiliensis; 10 A 4 cfu/mL for Escherichia coli and Candida Albicans; 10 to 5 cfu /mL for Staphylococcus aureus and Pseudomonas aeruginosa. At the end of the inoculation, the inoculated media are again carefully homogenized by aspiration-discharge.
  • the samples inoculated with Aspergillus brasiliensis are incubated at 30° C. (+/- 2.5° C.) for 48 hours.
  • the samples inoculated with the other strains are incubated at 37°C (+/-2.5°C) for 48 hours.
  • Samples and counts of the microorganisms are carried out at 30 minutes, 24 hours and 48 hours for each microorganism.
  • the inoculated samples are taken, serially diluted in diluent (casein peptone 1 g/L, sodium chloride 8.5 g/L, pH 7) and deposited respectively on potato and dextrose agars for Aspergillus brasiliensis, tryptocasein-soya agars for Escherichia coli and Sabouraud dextrose agars for Candida albicans.
  • the agars are incubated for 24 to 72 hours before counting the colonies present.
  • the measurements of populations of microorganisms carried out at each sampling time are expressed in cfu/mL.
  • the detection limit of the test is 100 cfu/mL.
  • compositions 40 and 43 have antibacterial and antifungal properties under in vitro culture conditions on agar-type medium, because they make it possible to microbiologically stabilize culture media inoculated with bacteria and fungi. reference for periods of up to 48 hours.
  • the antimicrobial compositions retain their antifungal and antibacterial properties once incorporated into cosmetic compositions.
  • Example 4 activation of preservatives at pH 6 in an oil-in-water emulsion
  • composition 43 prepared in Example 3 to activate the bactericidal and fungicidal activity of preservatives at pH 6 in an oil-in-water emulsion is demonstrated.
  • the preservatives are phenoxyethanol, benzyl alcohol, sodium benzoate, and potassium sorbate. They are listed in appendix 5 of regulation no. 1223/2009.
  • the cosmetic product used for this demonstration is a cream of the oil-in-water emulsion type, called “cotton cream”.
  • Creams are prepared according to the composition of table 12, by adding sufficient quantities, denoted "Qs", of composition 43 and preservative according to the values of table 10.
  • phase A is mixed separately and heated to 75°C. While maintaining at 75° C., phase B is added to phase A with gentle stirring (500-750 rpm; marine propeller), and the mixture is waited for to be homogeneous. Then phase A+B is added to phase C with emulsifying stirring (3000 rpm; deflocculating) for 10 minutes, maintaining at 75°C. The mixture is allowed to cool to 45° C., and phase D is added with moderate stirring (1500 rpm; marine propeller). The mixture is cooled to 25° C. with gentle stirring (500-750 rpm; marine propeller), then the pH is finally adjusted to 6 with phase E.
  • Each antimicrobial protection efficacy test is conducted according to the guidelines of the ISO 11930:2019 standard. The results are provided in Tables 14 to 19. They are expressed as the logarithmic reduction in the number of colony forming units per mL. A positive value corresponds to a decrease in the number of colony forming units. A negative value corresponds to an increase in the number of colony forming units.
  • cream 1 which is a cream without any preservative and without preservative activator, shows that cream 1 is not protected against Pseudomonas Aeruginosa, Escherichia Coli, and Candida Albicans, but is protected against Staphylococcus Aureus and Aspergillus Brasiliensis (we speak of self-protection) beyond 14 days. This measurement is our negative control.
  • composition 43 contains 1% and 1.5% of composition 43 respectively, and no preservative, show that none of these creams is protected against Pseudomonas Aeruginosa and Candida Albicans. Self-protection against Staphylococcus Aureus and Aspergillus Brasiliensis is maintained. Concerning Escherichia Coli, protection is observed from 28 days. Composition 43 does not make it possible to protect the cream against microbial development. It is however notable that composition 43 does not degrade the self-protection of the cream against Staphylococcus Aureus and Aspergillus Brasiliensis.
  • cream 6 which contains 0.4% by weight of phenoxyethanol and 1% by weight of composition 43
  • the microbial protection against Pseudomonas Aeruginosa, Escherichia Coli, and Aspergillus brasiliensis is much better than that of the cream 5, and equivalent to the positive control. Indeed, from 7 days, or 14 days for Aspergillus Brasiliensis, strong logarithmic reductions are measured, and are greater than the reductions measured on cream 5 by at least 2 log.
  • composition 43 therefore makes it possible to activate the preservative power of phenoxyethanol against Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis and Staphylococcus aureus.
  • cream 8 which contains 0.4% by weight of benzyl alcohol and 1% by weight of composition 43, it is found that the microbial protection against Pseudomonas Aeruginosa, Escherichia Coli, and Staphylococcus Aureus is well better than that of cream 7, and equivalent to the positive control. Indeed, from 7 days, or 14 days, significant or strong logarithmic reductions are measured, and are greater than the reductions measured on cream 7, by at least 2 log for Pseudomonas Aeruginosa and Escherichia Coli and Staphylococcus Aureus. These reductions continue or are maintained at 14 days and 28 days. However, Cream 8 is not protected against Candida albicans, which continues to grow there.
  • composition 43 therefore makes it possible to activate the preservative power of benzyl alcohol against Pseudomonas Aeruginosa, Escherichia Coli, and Staphylococcus Aureus.
  • cream 10 which contains 0.4% by weight of sodium benzoate and 1% by weight of composition 43
  • the microbial protection against Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis and Candida albicans is much better than that of cream 9, and equivalent to the positive control. Indeed, from 7 days, or 14 days for A. brasiliensis, significant or strong logarithmic reductions are measured, and are greater than the reductions measured on cream 7 by at least 1 or 2 log. These reductions continue or are maintained at 14 days and 28 days. Self-protection against Staphylococcus aureus is maintained. It is noteworthy that the cream 10 here presents sufficient protection against Candida albicans.
  • Composition 43 therefore makes it possible to activate the preservative power of sodium benzoate against Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis, and Candida albicans.
  • the combination of 1% (by weight) of composition 43 and 0.4% (by weight) of the sodium benzoate makes it possible to stabilize the cream according to criterion B of standard ISO 11930:2019.
  • cream 12 which contains 0.4% by weight of potassium sorbate and 1% by weight of composition 43
  • the microbial protection against Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Candida Albicans and Aspergillus brasiliensis is much better than that of cream 11 , and even better than that of positive control cream 2 (containing 1% of Microcare® PM4).
  • positive control cream 2 containing 1% of Microcare® PM4
  • strong logarithmic reductions are measured, and are greater than the reductions measured on cream 11 by at least 2 log. These reductions are maintained or continue at 14 days and 28 days.
  • composition 43 therefore makes it possible to activate the preservative power of potassium sorbate against Pseudomonas Aeruginosa, Escherichia Coli, Candida Albicans, Staphylococcus Aureus and Aspergillus brasiliensis.
  • the combination of 1% (by weight) of composition 43 and 0.4% (by weight) of potassium sorbate makes it possible to stabilize the cream according to criterion A of standard ISO 11930:2019.
  • Example 5 cosmetic products comprising the “preservative activator” composition and a preservative
  • a shampoo is prepared according to the composition of table 22:
  • Antimicrobial protection efficacy tests are carried out on each shampoo in table 23 for the five microorganisms of the ISO 11930:2019 standard Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Candida Albicans, Aspergillus Brasiliensis. The results are shown in Table 24.
  • potassium sorbate which is a listed preservative, exerts a protective effect against three microorganisms Pseudomonas Aeruginosa, Candida Albicans and Aspergillus Brasiliensis, but destroys the self-protection of the formula against Escherichia Coli, making it non protected against this last bacterium.
  • composition 43 makes it possible to exert an antibacterial activity targeted on the Escherichia Coli strain effective from seven days and up to 28 days.
  • composition 43 thus makes it possible to protect the shampoo against the development of bacteria of the genus Escherichia Coli, and this without reducing or disturbing the antimicrobial activity of the preservative which is potassium sorbate, but on the contrary by activating the antimicrobial activity of potassium sorbate.

Abstract

The present application relates to the use of an antimicrobial composition essentially comprising natural ingredients as a preservative activator in cosmetic products. Due to the selection of the components of said antimicrobial composition, it has very broad compatibility with most cosmetic product formulations, and can, in particular, be integrated into said formulations without destabilising them or having to modify them, while maintaining the transparency of the cosmetic products.

Description

Description Description
Titre : composition liquide antimicrobienne et son utilisation comme activateur de conservateur de produits cosmétiques Title: antimicrobial liquid composition and its use as a preservative activator for cosmetic products
Domaine technique Technical area
[0001] L’invention relève du domaine de la conservation de produits cosmétiques, et plus précisément du domaine des activateurs de conservateur de produits cosmétiques. The invention relates to the field of the preservation of cosmetic products, and more specifically to the field of activators of preservatives for cosmetic products.
Technique antérieure Prior technique
[0002] Ces dernières années, la cosmétique fait face à une situation de plus en plus difficile dans un domaine tout aussi essentiel que l’efficacité des produits cosmétiques en elle-même : à savoir, la conservation des produits cosmétiques, au sens microbiologique du terme. Les produits cosmétiques sont des milieux aqueux propices au développement de bactéries, de champignons et de levures. Pour garantir la sécurité des consommateurs, des molécules ou composés ayant des activités antibactériennes et antifongiques doivent être ajoutés aux produits cosmétiques. La réglementation encadre strictement la nature de ces molécules ou composés, ainsi que les doses auxquels ils peuvent être ajoutés aux produits cosmétiques, comme par exemple en France dans le règlement cosmétique N° 1223/2009 en l’annexe 5 intitulé « liste des agents conservateurs admis dans les produits cosmétiques », qui compte soixante conservateurs autorisés. [0002] In recent years, cosmetics has been faced with an increasingly difficult situation in a field that is just as essential as the effectiveness of cosmetic products in themselves: namely, the preservation of cosmetic products, in the microbiological sense of the term. Cosmetic products are aqueous media conducive to the development of bacteria, fungi and yeasts. To ensure consumer safety, molecules or compounds with antibacterial and antifungal activities must be added to cosmetic products. The regulations strictly regulate the nature of these molecules or compounds, as well as the doses at which they can be added to cosmetic products, as for example in France in cosmetic regulation No. 1223/2009 in appendix 5 entitled "list of preservatives allowed in cosmetic products”, which has sixty authorized preservatives.
[0003] Dans les faits, le nombre de conservateurs autorisés qui sont réellement utilisés par les producteurs de produits cosmétiques est bien plus réduit, et proche d’une quinzaine de conservateurs. Les conservateurs faisant l’unanimité se comptent même sur les doigts d’une main. Les producteurs se limitent à ces conservateurs soit par anticipation de changements de réglementation, soit par besoin de satisfaire aux attentes des consommateurs de disposer de produits cosmétiques les plus propres ou les plus naturels possible. [0003] In fact, the number of authorized preservatives that are actually used by producers of cosmetic products is much smaller, and close to about fifteen preservatives. The unanimous conservatives can even be counted on the fingers of one hand. Producers limit themselves to these preservatives either in anticipation of regulatory changes, or out of a need to meet consumer expectations of having the cleanest or most natural cosmetic products possible.
[0004] Pour réussir à satisfaire cette attente des consommateurs, les producteurs de produits cosmétiques vont encore plus loin en essayant de réduire la quantité de conservateur à son minimum, voire même à une valeur inférieure à sa dose minimale requise connue, et en l’associant à d’autres molécules ou composés dits « activateur de conservateur » afin d’obtenir un effet de conservation. Ces « activateur de conservateur » ne sont pas des conservateurs listés en tant que tel, mais possèdent des activités, notamment antimicrobiennes, qui complètent ou augmentent l’activité antimicrobienne des conservateurs. [0004] To succeed in satisfying this consumer expectation, producers of cosmetic products go even further by trying to reduce the amount of preservative to its minimum, or even to a value lower than its known minimum required dose, and by combining it with other molecules or compounds called "preservative activator" in order to obtain a preservative effect. These "preservative activators" are not preservatives listed as such, but have activities, in particular antimicrobial, which supplement or increase the antimicrobial activity of the preservatives.
[0005] Les huiles essentielles sont largement connues pour leurs activités antibactériennes et antifongiques. De nombreux brevets ont tenté de les associer à d’autres ingrédients. [0005] Essential oils are widely known for their antibacterial and antifungal activities. Many patents have attempted to combine them with other ingredients.
[0006] Le brevet Lonza WO 2014/014416 enseigne des compositions antimicrobiennes composées d’un actif conservateur et d’un potentialisateur dudit actif. L’actif conservateur peut être choisi parmi une multitude de composés, allant du cinnamaldéhyde à l’acide sorbique ou acide benzoïque, et aux huiles essentielles de gaulthérie ou de citronnelle. Le potentialisateur peut être choisi parmi l’acide érythorbique ou l’acide gluconique, ou leurs sels. Concernant l’acide gluconique, sa forme cyclique, connue sous le nom de gluconolactone, est préférée. L’huile de citronnelle est citée dans cette demande, et les données d’activité antibactérienne présentées montrent que cette huile essentielle n’a pas une activité suffisante pour agir en conservateur ou activateur de conservateur. De nombreux additifs sont évoqués dans cette demande, parmi lesquels des solubilisants, sans qu’aucune indication ne soit donnée quant à leur nature ou leur utilité pour la composition ou pour la formulation cosmétique. [0006] Lonza patent WO 2014/014416 teaches antimicrobial compositions composed of a preservative active ingredient and a potentiator of said active ingredient. The preservative active can be chosen from a multitude of compounds, ranging from cinnamaldehyde to sorbic acid or benzoic acid, and essential oils of wintergreen or lemongrass. The potentiator can be chosen from erythorbic acid or gluconic acid, or their salts. Regarding gluconic acid, its cyclic form, known as gluconolactone, is preferred. Lemongrass oil is cited in this application, and the antibacterial activity data presented show that this essential oil does not have sufficient activity to act as a preservative or preservative activator. Many additives are mentioned in this application, including solubilizers, without any indication being given as to their nature or their usefulness for the composition or for the cosmetic formulation.
[0007] Le brevet CleanWell US6346281 propose de combiner l’huile essentielle de citronnelle avec des ions métalliques, tels que le sulfate de cuivre, et avec un « biosurfactant » et un solvant. Le « biosurfactant » peut être soit le « BOD », soit le Tween-80 qui est un sorbitane polyéthoxylé. Le solvant peut être choisi parmi les solvants organiques tels que l’éthanol. Selon un autre brevet Cleanwell WO 2010/059399, la combinaison d’huile de thym avec des ions cuivres Cu2+ et un alkylpolyglucoside permet d’obtenir une composition apte à mousser, utile pour le traitement et la prévention des infections bactériennes résistantes aux antibiotiques, notamment les souches de Staphylococcus aureus résistantes à la méthicilline. [0007] The CleanWell patent US6346281 proposes combining citronella essential oil with metal ions, such as copper sulphate, and with a “biosurfactant” and a solvent. The "biosurfactant" can be either "BOD" or Tween-80 which is a polyethoxylated sorbitan. The solvent can be chosen from organic solvents such as ethanol. According to another Cleanwell patent WO 2010/059399, the combination of thyme oil with copper ions Cu2+ and an alkylpolyglucoside makes it possible to obtain a composition capable of foaming, useful for the treatment and prevention of bacterial infections resistant to antibiotics, in particular methicillin-resistant strains of Staphylococcus aureus.
[0008] Le brevet Reckitt Benckiser US5403587 combine une huile essentielle de thym ou de citronnelle avec un acide gras éthoxylé, un acide carboxylique « nonoxynol-10 », ou un sel de sodium d’acide gras de coco, et avec un tensioactif et un solvant organique. Le tensioactif et le solvant organique sont essentiels pour fournir une composition sous forme liquide apte à être dispersée ou solubilisée. Le tensioactif peut être choisi parmi les tensioactifs anioniques ou amphotériques. Ces combinaisons présentent une activité anti-bactérienne sur S. Aureus et sur P. Aeruginosa. [0008] The Reckitt Benckiser patent US5403587 combines an essential oil of thyme or lemongrass with an ethoxylated fatty acid, a “nonoxynol-10” carboxylic acid, or a coconut fatty acid sodium salt, and with a surfactant and an organic solvent. The surfactant and the organic solvent are essential to provide a composition in liquid form capable of being dispersed or solubilized. The surfactant can be chosen from anionic or amphoteric surfactants. These combinations exhibit antibacterial activity on S. Aureus and on P. Aeruginosa.
[0009] Le brevet Procter & Gamble W02008/126057 dévoile des compositions antimicrobiennes pour le soin de la bouche. Elles comprennent un mélange d’huiles essentielles contenant des composés acycliques et des composés cycliques. L’ajout d’acide gluconique est conseillé pour son pouvoir chélatant des ions calcium situés sur les parois des bactéries, ce qui contribue à améliorer le pouvoir bactéricide de la composition. Comme additifs, la composition peut comprendre tous les tensioactifs, mais les tensioactifs anioniques, les tensioactifs cationiques, ou les tensioactifs zwitterioniques, sont les préférés. Les tensioactifs non ioniques sont aussi cités, et le brevet insiste sur les tensioactifs non ioniques préparés par condensation d’oxyde d’alkylènes, c’est-à-dire les tensioactifs non ioniques polyéthoxylés. [0009] The Procter & Gamble patent W02008/126057 discloses antimicrobial compositions for the care of the mouth. They include a mixture of essential oils containing acyclic compounds and cyclic compounds. The addition of gluconic acid is recommended for its chelating power of the calcium ions located on the walls of the bacteria, which contributes to improving the bactericidal power of the composition. As additives, the composition can include all surfactants, but anionic surfactants, cationic surfactants, or zwitterionic surfactants are preferred. Nonionic surfactants are also cited, and the patent emphasizes nonionic surfactants prepared by condensation of alkylene oxide, i.e. polyethoxylated nonionic surfactants.
[0010]lndusco US9687002 propose de mettre l’huile essentielle de citronnelle en microémulsion dans de l’eau additivée d’acide citrique, acide lactique ou acide acétique comme tampon pH. La microémulsion est obtenue grâce à au moins deux tensioactifs ayant un HLB entre 9 et 18, et ces tensioactifs peuvent être des tensioactifs non ioniques. La microémulsion permet d’obtenir une composition stable, c’est-à-dire restant macroscopiquement homogène, et transparente. [0010]Indusco US9687002 proposes putting lemongrass essential oil in a microemulsion in water with citric acid, lactic acid or acetic acid added as a pH buffer. The microemulsion is obtained thanks to at least two surfactants having an HLB between 9 and 18, and these surfactants can be nonionic surfactants. The microemulsion makes it possible to obtain a stable composition, i.e. remaining macroscopically homogeneous, and transparent.
[0011]L’Oreal FR3061010 divulgue des nanoémulsions d’huile essentielle obtenue par émulsification de ces huiles essentielles dans un mélange d’eau et de solvant organique hydrosoluble par des tensioactifs choisis parmi les tensioactifs anioniques, non ioniques, amphotères, zwitterioniques ou cationiques. Ces nanoémulsions sont préparées pour leur utilisation topique pour le traitement d’infections bactérienne ou fongique. L’huile essentielle de citronnelle est présentée bien qu’aucune activité antimicrobienne ne lui soit attribuée. Parmi les tensioactifs non ioniques, les alkylpolyglucosides sont les préférés, et particulièrement le caprylyl/capryl glucoside, comme le Oramix™ CG110 de Seppic. Dans l’unique exemple de ce brevet, l’Oramix™ CG110 est formulé avec dix huiles essentielles, de l’éthanol et de l’eau. La quantité d’Oramix™ CG110 utilisée y est de 0,05 % en poids par rapport au poids total de la formulation. De manière générale, L’Oréal FR3061010 recommande d’utiliser une quantité de tensioactif non ionique inférieure à 1 % en poids par rapport au poids total de la nanoémulsion. C’est la combinaison d’un tensioactif non ionique et d’éthanol qui permet d’obtenir une nanoémulsion. Cet état de nanoémulsion présente des avantages en termes de texture, de douceur au touché, et de transparence. [0011] L'Oreal FR3061010 discloses essential oil nanoemulsions obtained by emulsification of these essential oils in a mixture of water and water-soluble organic solvent with surfactants chosen from anionic, nonionic, amphoteric, zwitterionic or cationic surfactants. These nanoemulsions are prepared for their topical use for the treatment of bacterial or fungal infections. Lemongrass essential oil is presented although no antimicrobial activity is attributed to it. Among the nonionic surfactants, alkyl polyglucosides are preferred, and particularly caprylyl/capryl glucoside, such as Oramix™ CG110 from Seppic. In the unique example of this patent, Oramix™ CG110 is formulated with ten essential oils, ethanol and water. The amount of Oramix™ CG110 used therein is 0.05% by weight relative to the total weight of the formulation. In general, L'Oréal FR3061010 recommends using an amount of nonionic surfactant of less than 1% by weight relative to the total weight of the nanoemulsion. It is the combination of a nonionic surfactant and ethanol which makes it possible to obtain a nanoemulsion. This state of nanoemulsion has advantages in terms of texture, softness to the touch, and transparency.
[0012]Selon le brevet Nestec WO2012/072488 situé dans le domaine de l’alimentaire, la mise en émulsion des huiles essentielles permet d’augmenter leur efficacité ou de réduire la quantité d’huile essentielle nécessaire. Ce brevet utilise la gomme d’acacia comme émulsionnant pour former des émulsions d’huile essentielle dans de l’eau. [0012] According to the Nestec patent WO2012/072488 located in the field of food, the emulsification of essential oils makes it possible to increase their effectiveness or to reduce the quantity of essential oil necessary. This patent uses acacia gum as an emulsifier to form emulsions of essential oil in water.
[0013] Cependant, l’utilisation des huiles essentielles en tant qu’activateur de conservateur n’est pas simple, et nécessite d’apporter des solutions à plusieurs problèmes techniques. [0013] However, the use of essential oils as a preservative activator is not simple, and requires solutions to several technical problems.
[0014] En effet, les huiles essentielles sont des extraits naturels insolubles dans l’eau, connus depuis l’antiquité pour leurs activités antiseptiques, mais aussi pour leur potentiel caractère allergène, ce qui impose de trouver, pour leur usage en cosmétique, une dose équilibrée entre le besoin d’augmenter cette dose, pour augmenter l’activité antiseptique, et le besoin de réduire cette dose, pour ne pas provoquer d’allergie. De plus, il est généralement recherché que l’activité antiseptique ait un spectre le plus grand possible, afin de pouvoir inhiber la croissance ou tuer tous les micro-organismes, à savoir les bactéries, les champignons, les levures, et les virus. La recherche d’une dose équilibrée et d’un spectre d’activité large conduit souvent à utiliser un cocktail d’huiles essentielles à de très faibles doses, ou à combiner quelques huiles essentielles avec d’autres actifs antimicrobiens ou avec des composés potentialisant ou agissant en synergie avec les huiles essentielles. Cela va dans le sens de complexifier la composition antimicrobienne, et d’augmenter les risques d’interactions néfastes. [0014] Indeed, essential oils are natural extracts insoluble in water, known since antiquity for their antiseptic activities, but also for their potential allergenicity, which requires finding, for their use in cosmetics, a dose balanced between the need to increase this dose, to increase the antiseptic activity, and the need to reduce this dose, so as not to cause an allergy. In addition, it is generally sought that the antiseptic activity has the widest possible spectrum, in order to be able to inhibit the growth or kill all microorganisms, namely bacteria, fungi, yeasts, and viruses. The search for a balanced dose and a broad spectrum of activity often leads to the use of a cocktail of essential oils at very low doses, or to the combination of a few essential oils with other antimicrobial active ingredients or with compounds that potentiate or acting in synergy with essential oils. This goes in the direction of making the antimicrobial composition more complex, and increasing the risks of harmful interactions.
[0015] De plus, la cosmétique moderne pose un problème supplémentaire à l’usage des huiles essentielles, à savoir le besoin de les rendre actives dans les formulations cosmétiques comprenant une phase aqueuse, et une multitude d’ingrédients susceptibles d’interagir négativement avec l’huile essentielle. Pour exercer son activité antimicrobienne dans la phase aqueuse, il convient que l’huile essentielle soit dispersée finement ou solubilisée dans cette phase aqueuse. Cette dispersion ou cette solubilisation sont généralement faites, a minima, en ajoutant un tensioactif solubilisant, et plus avantageusement, en ajoutant en plus un solvant organique hydrosoluble, à la formulation du produit cosmétique. Toutes les catégories de tensioactifs solubilisants ont été envisagés par l’art antérieur. [0015] In addition, modern cosmetics poses an additional problem for the use of essential oils, namely the need to make them active in cosmetic formulations comprising an aqueous phase, and a multitude of ingredients likely to interact negatively with essential oil. To exert its antimicrobial activity in the aqueous phase, the essential oil should be finely dispersed or dissolved in this aqueous phase. This dispersion or this solubilization are generally made, at least, by adding a solubilizing surfactant, and more advantageously, by adding an organic solvent. water-soluble, to the formulation of the cosmetic product. All categories of solubilizing surfactants have been considered by the prior art.
[0016]Toutefois, si des combinaisons de tensioactifs solubilisants et d’huiles essentielles ont pu montrer leur efficacité antimicrobienne, l’incorporation de telles associations dans des formulations cosmétiques a pu déstabiliser les formulations et provoquer notamment des déphasages ou la formation de particules solides. [0016] However, if combinations of solubilizing surfactants and essential oils have been able to show their antimicrobial efficacy, the incorporation of such combinations into cosmetic formulations has been able to destabilize the formulations and in particular cause phase shifts or the formation of solid particles.
[0017] Par ailleurs, la composition d’un produit cosmétique est très différente de celle d’un milieu de culture de test in-vitro. Dans un produit cosmétique, des interactions entre les constituants de la composition antimicrobienne et les ingrédients du produit cosmétique peuvent survenir, résultant en l’altération ou la suppression de l’activité antimicrobienne. Il peut alors s’avérer nécessaire d’augmenter la dose en composition antimicrobienne pour retrouver l’activité antimicrobienne in-situ. [0017] Furthermore, the composition of a cosmetic product is very different from that of an in-vitro test culture medium. In a cosmetic product, interactions between the constituents of the antimicrobial composition and the ingredients of the cosmetic product may occur, resulting in the alteration or suppression of the antimicrobial activity. It may then be necessary to increase the dose of antimicrobial composition to regain the antimicrobial activity in situ.
Problème technique Technical problem
[0018]Ainsi, il est nécessaire de trouver un activateur de conservateur composé de produits naturels ou de produits d’origine naturelle, biodégradable, dépourvu de composés éthoxylés ou siliconés, transparent et qui puisse être intégré dans un produit cosmétique sans altérer les propriétés physico-chimiques du produit, c’est-à-dire sans altérer ou déstabiliser le produit cosmétique, ni provoquer de déphasage ou la formation de particules solides, et ce pour la majorité des formes galéniques. Il est aussi également nécessaire de mettre au point une formulation qui préserve les propriétés antimicrobiennes de l’activateur. [0018] Thus, it is necessary to find a preservative activator composed of natural products or products of natural origin, biodegradable, devoid of ethoxylated or silicone compounds, transparent and which can be integrated into a cosmetic product without altering the physical properties -chemicals of the product, that is to say without altering or destabilizing the cosmetic product, or causing a phase shift or the formation of solid particles, and this for the majority of dosage forms. It is also necessary to develop a formulation that preserves the antimicrobial properties of the activator.
Brève description des dessins Brief description of the drawings
[0019] D’autres caractéristiques, détails et avantages de l’invention apparaîtront à la lecture de la description détaillée ci-après, et à l’analyse des dessins annexés, sur lesquels : Other characteristics, details and advantages of the invention will appear on reading the detailed description below, and on analyzing the appended drawings, in which:
Fig. 1 Fig. 1
[0020][Fig. 1 ] montre les résultats des tests d’activité antimicrobienne de la composition liquide antimicrobienne sur Escherichia coli ATCC® 8739. [0020][Fig. 1] shows the results of antimicrobial activity testing of the antimicrobial liquid composition on Escherichia coli ATCC® 8739.
Fig. 2 [0021][Fig. 2] montre les résultats des tests d’activité antimicrobienne de la composition liquide antimicrobienne sur Candida albicans ATCC® 10231. Fig. 2 [0021][Fig. 2] shows the results of antimicrobial activity testing of the antimicrobial liquid composition against Candida albicans ATCC® 10231.
Fig. 3 Fig. 3
[0022] [Fig. 3] montre les résultats des tests d’activité antimicrobienne de la composition liquide antimicrobienne sur Aspergillus brasiliensis ATCC® 16404. [0022] [Fig. 3] shows the results of antimicrobial activity testing of the antimicrobial liquid composition against Aspergillus brasiliensis ATCC® 16404.
Fig. 4 Fig. 4
[0023] [Fig. 4] montre les résultats des tests d’activité antimicrobienne de la composition liquide antimicrobienne sur Staphylococcus aureus ATCC® 6538. [0023] [Fig. 4] shows the results of antimicrobial activity testing of the antimicrobial liquid composition against Staphylococcus aureus ATCC® 6538.
Fig. 5 Fig. 5
[0024] [Fig. 5] montre les résultats des tests d’activité antimicrobienne de la composition liquide antimicrobienne sur Pseudomonas aeruginosa ATCC® 9027.[0024] [Fig. 5] shows the results of antimicrobial activity testing of the antimicrobial liquid composition against Pseudomonas aeruginosa ATCC® 9027.
Résumé de l’invention Summary of the invention
[0025] La Demanderesse a démontré que des compositions antimicrobiennes selon l’invention permettaient d’activer les conservateurs et d’augmenter leur protection antimicrobienne. En effet, de fortes réductions logarithmiques du nombre d’unités formant colonies de Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans et Staphylococcus Aureus sont mesurées lorsque les compositions antimicrobiennes sont introduites dans la composition cosmétique, en association avec un conservateur, et ce comparativement à une composition cosmétique ne comprenant qu’un conservateur usuellement utilisé. The Applicant has demonstrated that antimicrobial compositions according to the invention make it possible to activate preservatives and increase their antimicrobial protection. In fact, strong logarithmic reductions in the number of colony-forming units of Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans and Staphylococcus Aureus are measured when the antimicrobial compositions are introduced into the cosmetic composition, in combination with a preservative, and this compared to a cosmetic composition comprising only a preservative usually used.
[0026]Ainsi, la présente invention concerne l’utilisation d’une composition liquide antimicrobienne pour activer les conservateurs de produits cosmétiques, ladite composition liquide antimicrobienne comprenant : [0026] Thus, the present invention relates to the use of an antimicrobial liquid composition for activating the preservatives of cosmetic products, said antimicrobial liquid composition comprising:
- Au moins une huile essentielle choisie parmi les huiles essentielles d’espèces du genre Cymbopogon, les huiles essentielles de clou de girofle, de géranium Bourbon, de laurier noble, de litsée citronnée, de mélisse, de piment, de piment couronné, d’origan, d’arbre à thé, de thym, de schénanthe ; - At least one essential oil chosen from the essential oils of species of the genus Cymbopogon, the essential oils of clove, Bourbon geranium, noble laurel, lemony litsea, lemon balm, pepper, crown pepper, oregano, tea tree, thyme, lemongrass;
- Au moins un tensioactif non-ionique choisi parmi les alkyl(poly)glycosides, les alkylglycosides, les esters d’huiles végétales, les esters gras non éthoxylés de polyols, les hétéropolymères d’alkylglycosides en C8-C10 et d’esters gras de sorbitan, ou leurs mélanges, - At least one nonionic surfactant chosen from alkyl(poly)glycosides, alkylglycosides, esters of vegetable oils, non-ethoxylated fatty esters of polyols, heteropolymers of C8-C10 alkylglycosides and sorbitan fatty esters, or mixtures thereof,
Au moins un acide carboxylique sous forme libre. At least one carboxylic acid in free form.
[0027] La présente invention concerne également des compositions antimicrobiennes comprenant The present invention also relates to antimicrobial compositions comprising
- de l’huile essentielle d’une des espèces du genre Cymbopogon, - essential oil of one of the species of the genus Cymbopogon,
- du caprylyl/capryl glucoside, - caprylyl/capryl glucoside,
- de l’acide gluconique, - gluconic acid,
- du gluconate de sodium, - sodium gluconate,
- de l’eau. - some water.
[0028]Ces compositions permettent avantageusement de stabiliser les produits cosmétiques dans lesquels elles sont incorporées, sans altérer ou déstabiliser le produit cosmétique, ni provoquer de déphasage ou la formation de particules solides. Avantageusement encore, les compositions antimicrobiennes selon l’invention gardent leur activité antimicrobienne une fois formulée dans un produit cosmétique. [0028]These compositions advantageously make it possible to stabilize the cosmetic products in which they are incorporated, without altering or destabilizing the cosmetic product, or causing a phase shift or the formation of solid particles. Advantageously again, the antimicrobial compositions according to the invention keep their antimicrobial activity once formulated in a cosmetic product.
[0029]Ainsi, la présente invention concerne également des produits cosmétiques comprenant des compositions antimicrobiennes selon l’invention et au moins un conservateur. [0029] Thus, the present invention also relates to cosmetic products comprising antimicrobial compositions according to the invention and at least one preservative.
Description des modes de réalisation Description of embodiments
[0030]A des fins de clarté, dans la présente demande : [0030] For clarity, in the present application:
[0031]- l’expression « être composé de » aura le même sens que l’expression « comprendre », à savoir de définir une composition ouverte. [0031]- the expression "to be composed of" will have the same meaning as the expression "to understand", namely to define an open composition.
[0032]- les constituants autres que l’eau, de la composition antimicrobienne objet de la présente demande sont parfois commercialisés sous forme de solutions aqueuses, composées d’eau et d’un desdits constituants. Afin de se libérer de cette teneur en eau, qui peut varier selon les constituants et leurs fournisseurs, les pourcentages massiques en lesdits constituants autres que l’eau dans la composition antimicrobienne, exprimés en % en poids sec, sont les pourcentages massiques des masses sèches en lesdits constituants, autrement dit les pourcentages massiques en lesdits constituants secs, l’eau étant exclue. [0033]- la composition liquide antimicrobienne objet de la présente demande est une composition aqueuse. Les quantités de composition liquide antimicrobienne mises en œuvre sont exprimés en pourcentages massiques bruts, notés % en poids brut, rendant compte de la composition liquide antimicrobienne dans sa totalité, autrement dit en tenant compte de tous ses constituants, l’eau y compris. [0032] the constituents other than water of the antimicrobial composition that is the subject of the present application are sometimes marketed in the form of aqueous solutions, composed of water and one of said constituents. In order to get rid of this water content, which can vary according to the constituents and their suppliers, the mass percentages of said constituents other than water in the antimicrobial composition, expressed in% by dry weight, are the mass percentages of the dry masses into said constituents, in other words the mass percentages of said dry constituents, water being excluded. [0033]- the liquid antimicrobial composition which is the subject of the present application is an aqueous composition. The quantities of liquid antimicrobial composition used are expressed in gross mass percentages, denoted as % by gross weight, accounting for the antimicrobial liquid composition in its entirety, in other words taking into account all of its constituents, including water.
[0034] La présente invention concerne l’utilisation d’une composition liquide antimicrobienne pour activer les conservateurs de produits cosmétiques, ladite composition liquide antimicrobienne comprenant : The present invention relates to the use of an antimicrobial liquid composition for activating the preservatives of cosmetic products, said antimicrobial liquid composition comprising:
- Au moins une huile essentielle choisie parmi les huiles essentielles d’espèces du genre Cymbopogon, les huiles essentielles de clou de girofle, de géranium Bourbon, de laurier noble, de litsée citronnée, de mélisse, de piment, de piment couronné, d’origan, d’arbre à thé, de thym, de schénanthe ou un mélange de ces huiles; - At least one essential oil chosen from the essential oils of species of the genus Cymbopogon, the essential oils of clove, Bourbon geranium, noble laurel, lemony litsea, lemon balm, pepper, crown pepper, oregano, tea tree, thyme, lemongrass or a mixture of these oils;
- Au moins un tensioactif non-ionique choisi parmi les alkyl(poly)glycosides, les alkylglycosides, les alkylglycosides, les esters d’huiles végétales, les esters gras non éthoxylés de polyols, les hétéropolymères d’alkylglycosides en C8- C10 et d’esters gras de sorbitan, ou leurs mélanges, - At least one non-ionic surfactant chosen from alkyl (poly) glycosides, alkyl glycosides, alkyl glycosides, esters of vegetable oils, non-ethoxylated fatty esters of polyols, heteropolymers of C8-C10 alkylglycosides and sorbitan fatty esters, or mixtures thereof,
- Au moins un acide carboxylique sous forme libre. - At least one carboxylic acid in free form.
[0035] Selon un autre mode de réalisation, la présente invention concerne l’utilisation d’une composition liquide antimicrobienne pour activer les conservateurs de produits cosmétiques, ladite composition liquide antimicrobienne comprenant : According to another embodiment, the present invention relates to the use of an antimicrobial liquid composition to activate the preservatives of cosmetic products, said antimicrobial liquid composition comprising:
- Au moins une huile essentielle choisie parmi les huiles essentielles d’espèces du genre Cymbopogon, les huiles essentielles de clou de girofle, de géranium Bourbon, de laurier noble, de litsée citronnée, de mélisse, de piment, de piment couronné, d’origan, d’arbre à thé, de thym, de schénanthe ou mélange de ces huiles; - At least one essential oil chosen from the essential oils of species of the genus Cymbopogon, the essential oils of clove, Bourbon geranium, noble laurel, lemony litsea, lemon balm, pepper, crown pepper, oregano, tea tree, thyme, lemongrass or a mixture of these oils;
- Au moins un tensioactif non-ionique choisi parmi les alkyl(poly)glycosides,- At least one nonionic surfactant chosen from alkyl(poly)glycosides,
- Au moins un acide carboxylique sous forme libre. - At least one carboxylic acid in free form.
[0036] Activité antimicrobienne [0036] Antimicrobial activity
[0037]Au sens de l’invention, une composition antimicrobienne est une composition qui présente une activité antimicrobienne, c’est à dire que la composition est apte à ralentir la croissance d’au moins certaines bactéries, champignons ou levures, mieux à inhiber la croissance et à abaisser la présence en nombre d’au moins certains d’entre eux en les empêchant de se développer et de se multiplier, et mieux encore à rendre leur présence indécelable et à les faire totalement disparaître en les tuant. Par conséquent, la définition englobe un ralentissement de la croissance, une inhibition de croissance sous les termes connus de bactériostatique et de fongistatique, et aussi une activité létale, dite bactéricide ou fongicide. [0037] Within the meaning of the invention, an antimicrobial composition is a composition which exhibits antimicrobial activity, that is to say that the composition is capable of slowing down the growth of at least certain bacteria, fungi or yeasts, better at inhibiting the growth and lowering the presence in number of at least some of them by preventing them from developing and multiplying, and even better at make their presence undetectable and make them completely disappear by killing them. Therefore, the definition encompasses growth retardation, growth inhibition under the known terms bacteriostatic and fungistatic, and also lethal activity, known as bactericidal or fungicidal.
[0038] Activateur de conservateur de produit cosmétique [0038] Cosmetic product preservative activator
[0039]Mise en œuvre à des pourcentages massiques inférieurs à 5% en poids brut, voire 2,5% en poids brut, par rapport au poids total du produit cosmétique, la composition antimicrobienne selon l’invention s’avère par elle-même insuffisamment efficace à conserver un produit cosmétique (i.e. elle ne permet pas, de manière significative, de ralentir ou inhiber la croissance des bactéries ou champignons et ne possède pas d’activité bactéricide ou fongicide). [0039] Implemented at mass percentages of less than 5% by gross weight, or even 2.5% by gross weight, relative to the total weight of the cosmetic product, the antimicrobial composition according to the invention proves by itself insufficiently effective in preserving a cosmetic product (i.e. it does not significantly slow down or inhibit the growth of bacteria or fungi and does not have bactericidal or fungicidal activity).
[0040]Avantageusement, associée à un conservateur usuel, la composition antimicrobienne selon l’invention combine son activité antimicrobienne à l’activité dudit conservateur, et potentialise l’activité dudit conservateur. Il sera alors possible d’utiliser une dose réduite de conservateur, en association avec une dose appropriée de composition antimicrobienne, pour réussir à réduire la charge de micro-organismes dans le produit cosmétique, c’est-à-dire réduire le nombre d’unité formant colonie, voire préférentiellement à stabiliser la microbiologie du produit cosmétique selon la norme ISO 11930 :2019. La composition antimicrobienne permet ainsi effectivement de réduire la quantité de conservateur nécessaire pour conserver le produit cosmétique, et ce sur des durées équivalentes aux conservateurs usuels employés aux doses recommandées, qui sont généralement égales aux concentrations maximales admises dans les produits cosmétiques prêts à l’emploi. Les conservateurs dans les produits cosmétiques sont présents dans la composition cosmétique, soit seul, soit en combinaison, en une teneur d’environ 1 % en poids, par rapport au poids total de la composition. Comme démontré dans les exemples, les compositions antimicrobiennes selon l’invention permettent de diminuer la teneur en conservateur (par exemple 0.4% pour le sorbate de potassium et le benzoate de sodium), et de n’utiliser qu’un seul conservateur. [0041] Ainsi, un activateur de conservateur est un composé qui possède une activité antimicrobienne insuffisante en elle-même dans le produit cosmétique, mais qui est capable d’augmenter l’activité antimicrobienne d’un conservateur dans le produit cosmétique. On entend par « activité antimicrobienne insuffisante » un composé qui ne permet pas, de manière significative, de ralentir la croissance de bactéries, champignons ou levures, et encore moins d’inhiber leur croissance ou les tuer. L’activateur de conservateur ne peut donc pas stabiliser microbiologiquement un milieu par lui-même, et ne peut donc pas être qualifié de conservateur au sens de la réglementation. [0040] Advantageously, associated with a usual preservative, the antimicrobial composition according to the invention combines its antimicrobial activity with the activity of said preservative, and potentiates the activity of said preservative. It will then be possible to use a reduced dose of preservative, in combination with an appropriate dose of antimicrobial composition, to successfully reduce the load of microorganisms in the cosmetic product, that is to say reduce the number of colony-forming unit, or even preferentially to stabilize the microbiology of the cosmetic product according to the ISO 11930:2019 standard. The antimicrobial composition thus effectively makes it possible to reduce the quantity of preservative necessary to preserve the cosmetic product, and this over periods equivalent to the usual preservatives used at the recommended doses, which are generally equal to the maximum concentrations permitted in ready-to-use cosmetic products. . Preservatives in cosmetic products are present in the cosmetic composition, either alone or in combination, in a content of approximately 1% by weight, relative to the total weight of the composition. As demonstrated in the examples, the antimicrobial compositions according to the invention make it possible to reduce the preservative content (for example 0.4% for potassium sorbate and sodium benzoate), and to use only one preservative. [0041] Thus, a preservative activator is a compound which has insufficient antimicrobial activity by itself in the cosmetic product, but which is capable of increasing the antimicrobial activity of a preservative in the cosmetic product. The term “insufficient antimicrobial activity” means a compound which does not make it possible, in a significant manner, to slow down the growth of bacteria, fungi or yeasts, and even less to inhibit their growth or kill them. The preservative activator cannot therefore microbiologically stabilize a medium by itself, and therefore cannot be qualified as a preservative within the meaning of the regulations.
[0042] La combinaison d’un conservateur avec un activateur de conservateur permet donc de au moins augmenter l’activité antimicrobienne du conservateur et préférentiellement stabiliser microbiologiquement un produit cosmétique. Il est généralement recherché que cette stabilisation ou augmentation survienne à une dose en conservateur inférieure à la dose requise lorsque le conservateur est utilisé seul. The combination of a preservative with a preservative activator therefore makes it possible to at least increase the antimicrobial activity of the preservative and preferably to stabilize a cosmetic product microbiologically. It is generally desired that this stabilization or increase occur at a dose of preservative lower than the dose required when the preservative is used alone.
[0043] L’activité antimicrobienne peut être évaluée par toute méthode connue de l’homme du métier. The antimicrobial activity can be evaluated by any method known to those skilled in the art.
[0044] Le classement peut être fait par un suivi de la réduction du nombre d’unité formant colonie (noté ufc/mL) à sept, quatorze et vingt-huit jours après que le produit cosmétique ait été inoculé par un micro-organisme. La réduction du nombre d’unité formant colonie est exprimée en logarithme de base 10, par exemple un log de réduction correspond à une réduction de 10A1 , soit 10, ufc/mL, ou deux logs de réduction correspondent à une réduction de 10A2, soit 100, ufc/mL. The classification can be made by monitoring the reduction in the number of colony-forming units (denoted cfu/mL) at seven, fourteen and twenty-eight days after the cosmetic product has been inoculated with a microorganism. The reduction in the number of colony forming units is expressed in logarithm base 10, for example one log of reduction corresponds to a reduction of 10 A 1 , i.e. 10, cfu/mL, or two logs of reduction correspond to a reduction of 10 At 2, i.e. 100, cfu/mL.
[0045] Préférentiellement, l’activité antimicrobienne est évaluée selon la norme internationale ISO 11930 :2019 intitulée « ISO11930 Cosmétiques - Microbiologie - Evaluation de la protection antimicrobienne d’un produit cosmétique » qui spécifie un mode opératoire pour l'interprétation des données résultant de l'essai d'efficacité de la protection antimicrobienne et/ou de l'appréciation du risque microbiologique lors de l'évaluation globale de la protection antimicrobienne d'un produit cosmétique. Cette norme permet notamment de classer le niveau de protection microbiologique d’un produit cosmétique vis-à-vis des principaux pathogènes : les bactéries, à savoir Escherichia Coli, Staphylococcus Aureus, Pseudomonas Aeruginosa, et des champignons, à savoir Candida Albicans et Aspergillus Brasiliensis. [0046] Selon un mode de réalisation, une composition sera considérée comme activateur de conservateur lorsque, combinée au conservateur, elle permet d’augmenter d’au moins 1 log la réduction du nombre d’unités formant colonies de microorganismes présents dans le milieu, préférentiellement au moins deux logs, préférentiellement au moins 3 logs, comparativement au nombre d’unités formant colonies lorsque le conservateur seul est utilisé. Preferably, the antimicrobial activity is evaluated according to the international standard ISO 11930:2019 entitled "ISO11930 Cosmetics - Microbiology - Evaluation of the antimicrobial protection of a cosmetic product" which specifies a procedure for the interpretation of the data resulting from the test of the effectiveness of the antimicrobial protection and/or the assessment of the microbiological risk during the overall evaluation of the antimicrobial protection of a cosmetic product. This standard makes it possible in particular to classify the level of microbiological protection of a cosmetic product against the main pathogens: bacteria, namely Escherichia Coli, Staphylococcus Aureus, Pseudomonas Aeruginosa, and fungi, namely Candida Albicans and Aspergillus Brasiliensis . According to one embodiment, a composition will be considered as a preservative activator when, combined with the preservative, it makes it possible to increase by at least 1 log the reduction in the number of colony-forming units of microorganisms present in the medium, preferably at least two logs, preferably at least 3 logs, compared to the number of colony forming units when the preservative alone is used.
[0047] Selon un mode de réalisation, une composition sera considérée comme activateur de conservateur lorsque combinée au conservateur elle permet d’augmenter d’au moins 1 log la réduction du nombre d’unités formant colonies de microorganismes présents dans le milieu, préférentiellement au moins deux logs, préférentiellement au moins 3 logs, comparativement au nombre d’unités formant colonies de microorganismes lorsque le conservateur seul est utilisé, sur une période d’au moins 7 jours, préférentiellement 14 jours et encore préférentiellement sur une période d’au moins 28 jours. According to one embodiment, a composition will be considered as a preservative activator when combined with the preservative, it makes it possible to increase by at least 1 log the reduction in the number of units forming colonies of microorganisms present in the medium, preferentially to the at least two logs, preferably at least 3 logs, compared to the number of colony-forming units of microorganisms when the preservative alone is used, over a period of at least 7 days, preferably 14 days and even more preferably over a period of at least 28 days.
[0048] La composition liquide antimicrobienne objet de la présente demande peut être qualifiée de composition liquide à effet activateur de conservateur car elle satisfait à la définition précédente d’activateur de conservateur. De préférence, la composition liquide antimicrobienne est donc une composition liquide à effet activateur de conservateur. The antimicrobial liquid composition that is the subject of the present application can be qualified as a liquid composition with a preservative-activating effect because it satisfies the preceding definition of preservative-activating agent. Preferably, the antimicrobial liquid composition is therefore a liquid composition with a preservative-activating effect.
[0049]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer un conservateur et, combinée audit conservateur, de réduire d’au moins un log, préférentiellement au moins deux logs, préférentiellement au moins trois logs, le nombre d’unités formant colonies de Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans et de Staphylococcus aureus. According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate a preservative and, combined with said preservative, to reduce by at least one log, preferably at least two logs, preferably at least three logs, the number of colony forming units of Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans and Staphylococcus aureus.
[0050]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer un conservateur et, combinée audit conservateur, de réduire d’au moins un log, préférentiellement d’au moins deux logs, préférentiellement d’au moins 3 logs, le nombre d’unités formant colonies de Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans et de Staphylococcus aureus, sur une période d’au moins 7 jours, préférentiellement au moins 14 jours et préférentiellement au moins 28 jours. According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate a preservative and, combined with said preservative, to reduce by at least one log, preferentially by at least two logs, preferentially by at least 3 logs, the number of colony-forming units of Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis, Candida albicans and Staphylococcus aureus, over a period of at least 7 days, preferably at least 14 days and preferably at least 28 days.
[0051] Huile essentielle [0052]Selon un mode de réalisation, la composition antimicrobienne comprend une huile essentielle choisie parmi les huiles essentielles d’espèces du genre Cymbopogon, les huiles essentielles de clou de girofle, de géranium Bourbon, de laurier noble, de litsée citronnée, de mélisse, de piment, de piment couronné, d’origan, d’arbre à thé, de thym, de schénanthe ou un mélange de ces huiles. [0051] Essential oil [0052]According to one embodiment, the antimicrobial composition comprises an essential oil chosen from essential oils of species of the genus Cymbopogon, essential oils of clove, Bourbon geranium, noble laurel, lemon-litsea, lemon balm , chili, crown pepper, oregano, tea tree, thyme, lemongrass or a mixture of these oils.
[0053]Selon un mode de réalisation, l’huile essentielle est choisie parmi les huiles essentielles d’espèces du genre Cymbopogon. According to one embodiment, the essential oil is chosen from essential oils of species of the genus Cymbopogon.
[0054] Cymbopogon est un genre de plantes monocotylédones de la famille des Poaceae, sous-famille des Panicoideae, qui comprend une cinquantaine d'espèces originaires des régions tropicales et subtropicales d'Afrique, d'Asie et d'Australie. Ce sont des plantes herbacées, généralement vivaces, rarement annuelles, cespiteuses ou rhizomateuses, dont les tiges (chaumes) peuvent atteindre de 15 à 300 cm de long. [0054] Cymbopogon is a genus of monocotyledonous plants of the Poaceae family, Panicoideae subfamily, which comprises about fifty species originating from the tropical and subtropical regions of Africa, Asia and Australia. They are herbaceous plants, generally perennial, rarely annual, cespitose or rhizomatous, whose stems (culms) can reach 15 to 300 cm in length.
[0055] L’huile essentielle d’espèce du genre Cymbopogon est choisie parmi les huiles d’espèce du genre Cymbopogon riches en citral, en néral, en géranial et en géraniol. Préférentiellement, l’huile essentielle d’espèce du genre Cymbopogon est choisie parmi les huiles essentielles d’espèce du genre Cymbopogon présentant environ 30% en poids en néral, environ 40% en poids en géranial, et 5% en poids en géraniol. Ces pourcentages massiques sont usuellement déterminés par chromatographie. The essential oil of species of the genus Cymbopogon is chosen from oils of species of the genus Cymbopogon rich in citral, neral, geranial and geraniol. Preferably, the essential oil of species of the genus Cymbopogon is chosen from essential oils of species of the genus Cymbopogon having approximately 30% by weight in neral, approximately 40% by weight in geranial, and 5% by weight in geraniol. These mass percentages are usually determined by chromatography.
[0056] Parmi les huiles essentielles d’espèces du genre Cymbopogon, on peut citer : Among the essential oils of species of the Cymbopogon genus, mention may be made of:
- Cymbopogon citratus (DC.) Stapf., aussi appelée West indian lemongrass (en français : lemongrass de l’ouest de l’Inde) ou citronnelle des indes ou verveine des Indes, - Cymbopogon citratus (DC.) Stapf., also called West Indian lemongrass
- Cymbopogon flexuosus Stapf., aussi appelée East indian lemongrass (en français : lemongrass de l’est de l’Inde), - Cymbopogon flexuosus Stapf., also called East Indian lemongrass (in French: lemongrass de l’est de l’Inde),
- Cymbopogon nardus, aussi appelée citronnelle de Ceylan ou citronnelle de Sri Lanka, - Cymbopogon nardus, also called Ceylon lemongrass or Sri Lankan lemongrass,
- Cymbopogon nardus (L.) Watson, Cymbopogon nardus (L.) Rendel,- Cymbopogon nardus (L.) Watson, Cymbopogon nardus (L.) Rendel,
Cymbopogon schoenanthus (L), aussi appelée Camel grass ou geranium grass, Cymbopogon schoenanthus (L), also called Camel grass or geranium grass,
Cymbopogon winterianus Jowitt, aussi appelée citronnelle de Java - Cymbopogon martinii var. sofia, aussi appelée gingergrass, Cymbopogon winterianus Jowitt, also called Java Lemongrass - Cymbopogon martinii var. sofia, also called gingergrass,
- et Cymbopogon martinii var. motia., Cymbogopon maartinii roxb., aussi appelée palmarosa. - and Cymbopogon martinii var. motia., Cymbogopon maartinii roxb., also called palmarosa.
[0057]Selon un mode de réalisation, l’huile essentielle de Cymbopogon est choisie parmi les huiles essentielles des espèces Cymbopogon flexuosus Stapf. et Cymbopogon citratus (DC.) Stapf.. Tout préférentiellement, l’huile essentielle est une huile essentielle de citronnelle de l’espèce Cymbopogon citratus (DC.) Stapf. Typiquement, les huiles essentielles des espèces Cymbopogon flexuosus Stapf. et Cymbopogon citratus (DC.) Stapf. présentent environ 30% en poids en néral, environ 40% en poids en géranial, et 5% en poids en géraniol According to one embodiment, the Cymbopogon essential oil is chosen from the essential oils of the Cymbopogon flexuosus Stapf species. and Cymbopogon citratus (DC.) Stapf. Most preferably, the essential oil is an essential oil of citronella of the species Cymbopogon citratus (DC.) Stapf. Typically, essential oils of Cymbopogon flexuosus Stapf. and Cymbopogon citratus (DC.) Stapf. have about 30% by weight neral, about 40% by weight geranial, and 5% by weight geraniol
[0058]A titre d'exemple d'huiles essentielles d’espèces du genre Cymbopogon utiles à la composition liquide antimicrobienne objet de la présente demande, on peut citer celles commercialisées sous les dénominations « Cymbopogon flexuosus Oil® » par Elixens, et « HE Lemongrass citratus » d’origine Sri-Lanka par H. Reynaud & Fils. By way of example of essential oils of species of the genus Cymbopogon which are useful for the antimicrobial liquid composition which is the subject of the present application, mention may be made of those marketed under the names "Cymbopogon flexuosus Oil®" by Elixens, and "HE Lemongrass citratus” from Sri Lanka by H. Reynaud & Fils.
[0059] Parmi les huiles essentielles d’origan on citera l’origan à inflorescences, l’origan de Grèce, l’origan compact, l’origan vert, l’origan d'Espagne. Among the essential oils of oregano, mention will be made of inflorescence oregano, Greek oregano, compact oregano, green oregano, Spanish oregano.
[0060]Parmi les huiles essentielles de thym, on citera les huiles essentielles de thym sauvage, de thym à bornéol, de thym à carvacrol, de thym à linalol, de thym à thujanol, de thym à thymol, [0060]Among the essential oils of thyme, mention will be made of the essential oils of wild thyme, borneol thyme, carvacrol thyme, linalool thyme, thujanol thyme, thymol thyme,
[0061] L’huile essentielle peut aussi être choisie avantageusement parmi d’autres huiles riches en citral, en néral, en géranial et en géraniol. The essential oil can also be advantageously chosen from other oils rich in citral, neral, geranial and geraniol.
[0062] Il peut s’agir par exemple d’huile essentielle de litsée citronnée qui contient environ 40 % en poids de géranial et environ 30% en poids de néral ou d’huile essentielle de mélisse de l’espèce Melissa officinalis, par rapport au poids total d’huile essentielle. [0062] It may be, for example, essential oil of lemon bedsea which contains approximately 40% by weight of geranial and approximately 30% by weight of neral or essential oil of lemon balm of the species Melissa officinalis, compared to the total weight of essential oil.
[0063] Il peut s’agir aussi d’une huile essentielle riche en géraniol et en géranial comme en particulier l’huile essentielle de palmarosa (Cymbopogon martini) qui contient d’ordinaire entre 80% à 85 % en poids de géraniol par rapport au poids total d’huile essentielle. [0063] It may also be an essential oil rich in geraniol and geraniol, such as in particular the essential oil of palmarosa (Cymbopogon martini) which usually contains between 80% and 85% by weight of geraniol relative to the total weight of essential oil.
[0064]Selon un mode de réalisation, l’huile essentielle comprendra au moins une molécule active choisie parmi les molécules actives qui composent l’huile essentielle de lemongrass de l’espèce Cymbopogon flexuosus et Cymbopogon citratus : l’isomère trans du citral, connu sous le nom de géranial ou citral A, de nom IIICPA (E)-3,7- Dimethylocta-2,6-dienal ; l’isomère cis du citral, connu sous le nom de néral, ou citral B, de nom IIICPA (Z)-3,7-Dimethylocta-2,6-dienal ; le géraniol, de nom IIICPA (2E)- 3,7-diméthylocta-2,6-dién-1 -ol. [0064]According to one embodiment, the essential oil will comprise at least one active molecule chosen from the active molecules that make up the essential oil lemongrass of the species Cymbopogon flexuosus and Cymbopogon citratus: the trans isomer of citral, known as geranial or citral A, with the name IIICPA (E)-3,7-Dimethylocta-2,6-dienal; the cis isomer of citral, known as neral, or citral B, of the name IIICPA (Z)-3,7-Dimethylocta-2,6-dienal; geraniol, named IIICPA (2E)-3,7-dimethylocta-2,6-dien-1-ol.
[0065]Ainsi, selon un mode de réalisation, l’huile essentielle est choisie parmi les huiles essentielles de Cymbopogon, de litsée citronnée, de mélisse. [0065]Thus, according to one embodiment, the essential oil is chosen from the essential oils of Cymbopogon, lemon-litsea, lemon balm.
[0066]Selon un autre mode de réalisation, l’huile essentielle utile à la composition antimicrobienne objet de la présente demande peut être choisie parmi les huiles essentielles de l'ajowan (aussi appelé thym indien), d’anis étoilée (aussi appelé badiane), de basilic, de cannelle de Chine ou de Ceylan, de cardamome, de cyprès de Provence, d’eucalyptus citronné, d’eucalyptus globulus, d’eucalyptus radié, d’épinette noire, d’estragon, de fenouil, de gaulthérie, de genévrier de Virginie, de géranium grass, de géranium rosat, de géranium Bourbon, de gingergrass, de girofle (giroflier), d’inule odorante, de laurier noble, de lavandin reydovan, de lavande fine, de lavande aspic à cinéole, de lavande vraie, de lavandin, de lavandin super, de marjolaine des jardins, de marjolaine à coquilles, de melaleuque à feuilles linéaires, de menthe des champs, de menthe poivrée, de mélisse, de myrte rouge, de néroli, de niaouli, de petit grain bigarade, de pin sylvestre, de ravintsara (aussi appelée ravintsare ou camphrier de Madagascar), de romarin cinéole, de romarin camphré, de romarin officinal, de saro, de sarriette des jardins, de sarriette des montagnes, de schénanthe, de serpolet, de verveine exotique, de verveine des Indes, ou un mélange de ces huiles. According to another embodiment, the essential oil useful for the antimicrobial composition that is the subject of the present application can be chosen from the essential oils of ajwain (also called Indian thyme), star anise (also called star anise ), basil, Chinese or Ceylon cinnamon, cardamom, cypress from Provence, lemon eucalyptus, eucalyptus globulus, eucalyptus radiata, black spruce, tarragon, fennel, wintergreen , Virginia juniper, grass geranium, rose geranium, Bourbon geranium, gingergrass, clove (clove), fragrant inula, noble laurel, reydovan lavandin, fine lavender, cineole aspic lavender, true lavender, lavandin, super lavandin, garden marjoram, shell marjoram, linear-leaved tea tree, field mint, peppermint, lemon balm, red myrtle, neroli, niaouli, petit grain bigarade, Scots pine, ravintsara (also called ravintsara ntsare or Madagascar camphor), cineole rosemary, camphor rosemary, officinal rosemary, saro, garden savory, mountain savory, lemongrass, thyme, exotic verbena, Indian verbena, or a mixture of these oils.
[0067] L’huile essentielle pourra également être une huile riche en phénols, en particulier en carvacrol (présent par exemple dans l’huile essentielle de la sarriette), en thymol (présent par exemple dans l’huile essentielle de thym à thymol) et en eugénol (présent par exemple dans l’huile essentielle de clou de girofle). Ces phénols sont responsables des activités fongicides et bactéricides des huiles essentielles qui en contiennent. On peut citer plus particulièrement comme huiles riches en phénols, les huiles essentielles de thym (Thymus mastichina, Thymus vulgaris, Thymus zygis, Thymus thymi), de piment (Pimenta racemosa, Pimenta acris), d’ajowan (Trachyspermum ammi), de giroflier (Eugenia caryophyllus), de sarriette des montagnes (Satureja montana), d’origan (Origanum heracleoticum (Origan de Grèce), Origanum majorana, Origanum vulgare, Origanum compactum (Origan compact), d’origan d'espagne (Corydothymus capitatus), de cannelle de Ceylan (Cinnamomum verum). The essential oil may also be an oil rich in phenols, in particular in carvacrol (present for example in the essential oil of savory), in thymol (present for example in the essential oil of thyme with thymol) and in eugenol (present for example in clove essential oil). These phenols are responsible for the fungicidal and bactericidal activities of the essential oils that contain them. Mention may more particularly be made, as oils rich in phenols, of the essential oils of thyme (Thymus mastichina, Thymus vulgaris, Thymus zygis, Thymus thymi), pepper (Pimenta racemosa, Pimenta acris), ajowan (Trachyspermum ammi), clove (Eugenia caryophyllus), mountain savory (Satureja montana), oregano (Origanum heracleoticum (Greek oregano), Origanum majorana, Origanum vulgare, Origanum compactum (Oregano compact), Spanish oregano (Corydothymus capitatus), Ceylon cinnamon (Cinnamomum verum).
[0068]Selon un mode de réalisation, l’huile essentielle comprendra au moins une molécule active choisie parmi les monoterpénols, qui sont des alcools avec 10 atomes de carbone, préférentiellement le géraniol, le linalool, le thujanol, le myrcénol, le terpinéol, le menthol et le pipéritol. Les huiles essentielles qui comprennent ces molécules actives sont les huiles essentielles de palmarosa Cymbopogon martinii, de lavande aspic Lavandula spica, de menthe poivrée Mentha piperita, de marjolaine à coquilles Origanum majorana, et de « tea tree » (arbre à thé) de l’espèce Melaleuca alternifolia. According to one embodiment, the essential oil will comprise at least one active molecule chosen from monoterpenols, which are alcohols with 10 carbon atoms, preferably geraniol, linalool, thujanol, myrcenol, terpineol, menthol and piperitol. Essential oils that include these active molecules are palmarosa Cymbopogon martinii, spike lavender Lavandula spica, peppermint Mentha piperita, marjoram Origanum majorana, and tea tree essential oils. species Melaleuca alternifolia.
[0069]Selon un mode de réalisation, une autre huile essentielle pauvre en au moins un phénol, monoterpénol, oxyde de terpène, aldéhyde aromatiques, aldéhyde terpénique, phénylpropène, hydrocarbure monoterpénique, et hydrocarbure sesquiterpénique, peut être ajoutée à la composition objet de la présente demande, par exemple pour la parfumer, changer son odeur ou agir sur son activité antimicrobienne. Elle peut être choisie parmi l'huile essentielle de cèdre, l'huile essentielle d'orange douce, l'huile essentielle de citron, l'huile essentielle de mandarine verte ou rouge, ou l'huile essentielle de gaulthérie. According to one embodiment, another essential oil poor in at least one phenol, monoterpenol, terpene oxide, aromatic aldehyde, terpene aldehyde, phenylpropene, monoterpene hydrocarbon, and sesquiterpene hydrocarbon, can be added to the composition object of the present application, for example to perfume it, change its smell or act on its antimicrobial activity. It can be chosen from essential oil of cedar, essential oil of sweet orange, essential oil of lemon, essential oil of green or red mandarin, or essential oil of wintergreen.
[0070] La quantité totale d’huiles essentielles présente dans la composition liquide antimicrobienne peut aller de 0,1 % à 10% en poids sec, préférentiellement de 0,5% à 7% en poids sec, plus préférentiellement de 1 % à 5% en poids sec, et tout préférentiellement de 1 ,5% à 3% en poids sec, par rapport au poids total de la composition liquide antimicrobienne. The total quantity of essential oils present in the antimicrobial liquid composition can range from 0.1% to 10% by dry weight, preferentially from 0.5% to 7% by dry weight, more preferentially from 1% to 5 % by dry weight, and most preferably from 1.5% to 3% by dry weight, relative to the total weight of the antimicrobial liquid composition.
[0071] Le rapport de la masse sèche totale de tensioactifs non ioniques sur la masse sèche totale d’huiles essentielles peut en outre être supérieur ou égal à 2, préférentiellement supérieur ou égale à 3, plus préférentiellement supérieur ou égale à 4, et tout préférentiellement supérieur ou égal à 5. La ou les huiles essentielles sont avantageusement présentes dans la composition antimicrobienne en une quantité qui est en défaut par rapport à la quantité de ou des tensioactifs non ioniques. La sélection de cette situation de défaut permet de solubiliser au mieux la ou les huiles essentielles dans l’eau de la composition liquide antimicrobienne, et contribue aussi à maintenir cette solubilisation dans l’eau du produit cosmétique lorsque ladite composition liquide antimicrobienne est diluée dans ledit produit cosmétique, et notamment dans l’eau dudit produit cosmétique. The ratio of the total dry mass of nonionic surfactants to the total dry mass of essential oils may also be greater than or equal to 2, preferably greater than or equal to 3, more preferably greater than or equal to 4, and any preferably greater than or equal to 5. The essential oil(s) are advantageously present in the antimicrobial composition in a quantity which is lacking with respect to the quantity of nonionic surfactant(s). The selection of this default situation makes it possible to best solubilize the essential oil or oils in the water of the antimicrobial liquid composition, and also contributes to maintaining this solubilization in the water of the cosmetic product when the said liquid composition antimicrobial is diluted in said cosmetic product, and in particular in the water of said cosmetic product.
[0072]Ce rapport permet avantageusement, d’obtenir une composition liquide antimicrobienne stable, sans déphasage ou précipitation dans le temps, tout en étant transparente ou opalescente, à l’état concentré ou même après dilution élevé dans l’eau. This ratio advantageously makes it possible to obtain a stable antimicrobial liquid composition, without phase shift or precipitation over time, while being transparent or opalescent, in the concentrated state or even after high dilution in water.
[0073] Tensioactifs non-ioniques [0073] Nonionic surfactants
[0074]Selon un mode de réalisation, le tensioactif non ionique est choisi parmi : According to one embodiment, the nonionic surfactant is chosen from:
- les alcools, les alpha-diols et les alkyl(C1-C20)phénols, ces composés étant polyéthoxylés et/ou polypropoxylés et/ou polyglycérolés, le nombre de groupements oxyde d'éthylène et/ou oxyde de propylène pouvant aller de 1 à 100, et le nombre de groupements glycérol pouvant aller de 2 à 30; ou bien ces composés comprenant au moins une chaîne grasse comportant de 8 à 40 atomes de carbone, notamment de 16 à 30 atomes de carbone ; en particulier les alcools comprenant au moins une chaîne alkyle en C8 à C40, saturés ou non, linéaires ou ramifiés, oxyéthylénés comprenant de 1 à 100 moles d'oxyde d'éthylène, de préférence de 2 à 50, plus particulièrement de 2 à 40 moles d'oxyde d'éthylène et comportant une ou deux chaînes grasses;- alcohols, alpha-diols and (C1-C20)alkylphenols, these compounds being polyethoxylated and/or polypropoxylated and/or polyglycerolated, the number of ethylene oxide and/or propylene oxide groups possibly ranging from 1 to 100, and the number of glycerol groups possibly ranging from 2 to 30; or alternatively these compounds comprising at least one fatty chain comprising from 8 to 40 carbon atoms, in particular from 16 to 30 carbon atoms; in particular alcohols comprising at least one C8 to C40 alkyl chain, saturated or not, linear or branched, oxyethylenated comprising from 1 to 100 moles of ethylene oxide, preferably from 2 to 50, more particularly from 2 to 40 moles of ethylene oxide and comprising one or two fatty chains;
- les condensats d'oxyde d'éthylène et d'oxyde de propylène sur des alcools gras;- condensates of ethylene oxide and propylene oxide with fatty alcohols;
- les amides gras polyéthoxylés ayant de préférence de 2 à 30 motifs d'oxyde d'éthylène, les amides gras polyglycérolés comportant en moyenne de 1 à 5 groupements glycérol et en particulier de 1 ,5 à 4; - polyethoxylated fatty amides preferably having from 2 to 30 ethylene oxide units, polyglycerolated fatty amides comprising on average from 1 to 5 glycerol groups and in particular from 1.5 to 4;
- les esters d'acides gras du sorbitane éthoxylés ayant de préférence de 2 à 40 motifs d'oxyde d'éthylène ; - ethoxylated sorbitan fatty acid esters preferably having from 2 to 40 ethylene oxide units;
- les esters d'acides gras du saccharose ; - sucrose fatty acid esters;
- les esters d'acides gras polyoxyalkylénés, de préférence polyoxyéthylénés ayant de 2 à 150 moles d'oxyde d'éthylène dont les huiles végétales oxyéthylénées ; - polyoxyalkylenated fatty acid esters, preferably polyoxyethylenated, having from 2 to 150 moles of ethylene oxide, including oxyethylenated vegetable oils;
- les dérivés de N-(alkyl en C6-C24)glucamine, - N-(C6-C24 alkyl)glucamine derivatives,
- les oxydes d'amines tels que les oxydes d'(alkyl en C10-C14)amines ou les oxydes de N-(acyl en C10-C14)-aminopropylmorpholine ; - les esters gras non éthoxylés de polyols, et notamment parmi les esters gras non éthoxylés de glycérol, de polyglycérols, de sorbitol, de sorbitan, d’anydrodrohexitols comme en particulier l’isosorbide, de mannitol, de xylitol, d’érythritol, de maltitol, de saccharose, de glucose, de polydextrose, de sirops de glucose hydrogéné, de dextrines et d’amidons hydrolysés, - amine oxides such as (C10-C14 alkyl)amine oxides or N-(C10-C14 acyl)-aminopropylmorpholine oxides; - non-ethoxylated fatty esters of polyols, and in particular from non-ethoxylated fatty esters of glycerol, polyglycerols, sorbitol, sorbitan, androdrohexitols such as in particular isosorbide, mannitol, xylitol, erythritol, maltitol, sucrose, glucose, polydextrose, hydrogenated glucose syrups, dextrins and hydrolyzed starches,
- les esters de polyglycérol et d’acide gras saturés ou insaturés en C4-C20, préférentiellement en C8-C18, et plus préférentiellement en C18, par exemple le polyglyceryl-2 dipolyhydroxystearate et le polyglyceryl-3 diisostearate, - esters of polyglycerol and saturated or unsaturated C4-C20 fatty acids, preferably C8-C18, and more preferably C18, for example polyglyceryl-2 dipolyhydroxystearate and polyglyceryl-3 diisostearate,
- les esters d’huiles végétales, notamment parmi les esters d’huile de coco, par exemple le coco-caprylate, et leurs mélanges. - vegetable oil esters, in particular from coconut oil esters, for example coco-caprylate, and mixtures thereof.
[0075]Selon un autre mode de réalisation, le tensioactif non ionique est choisi parmi les alkyl(poly)glycosides, qui sont représentés par la formule générale suivante :According to another embodiment, the nonionic surfactant is chosen from alkyl(poly)glycosides, which are represented by the following general formula:
RiO-(R20)t-(G)v dans laquelle: RiO-(R 2 0)t-(G)v in which:
- Ri représente : un radical alkyle ou alcényle linéaire ou ramifié comportant 6 à 24 atomes de carbone, ou 6 à 18 atomes de carbone, ou de 6 à 12 atomes de carbone ; ou un radical alkylphényle dont le radical alkyle linéaire ou ramifié comporte 6 à 24 atomes de carbone, ou 6 à 18 atomes de carbone, ou de 6 à 12 atomes de carbone,- Ri represents: a linear or branched alkyl or alkenyl radical containing 6 to 24 carbon atoms, or 6 to 18 carbon atoms, or 6 to 12 carbon atoms; or an alkylphenyl radical whose linear or branched alkyl radical contains 6 to 24 carbon atoms, or 6 to 18 carbon atoms, or 6 to 12 carbon atoms,
- R2 représente un radical alkylène comportant 2 à 4 atomes de carbone, - R 2 represents an alkylene radical containing 2 to 4 carbon atoms,
- G représente un motif sucre comportant 5 à 6 atomes de carbone, - G represents a sugar unit comprising 5 to 6 carbon atoms,
- 1 désigne une valeur allant de 0 à 10, de préférence de 0 à 4, - 1 denotes a value ranging from 0 to 10, preferably from 0 to 4,
- v désigne une valeur allant de 1 à 15, de préférence de 1 à 4. - v denotes a value ranging from 1 to 15, preferably from 1 to 4.
[0076] De préférence, les tensioactifs alkyl(poly)glycoside sont des composés de formule décrite ci-dessus dans laquelle : Preferably, the alkyl(poly)glycoside surfactants are compounds of the formula described above in which:
- Ri désigne un radical alkyle saturé ou insaturé, linéaire ou ramifié comportant de 6 à 18 atomes de carbone, ou de 6 à 12 atomes de carbone, - Ri denotes a saturated or unsaturated, linear or branched alkyl radical comprising from 6 to 18 carbon atoms, or from 6 to 12 carbon atoms,
- R2 représente un radical alkylène comportant 2 à 4 atomes de carbone, - R 2 represents an alkylene radical containing 2 to 4 carbon atoms,
- 1 désigne une valeur allant de 0 à 3, de préférence égale à 0, - G désigne le glucose, le fructose ou le galactose, de préférence le glucose; - 1 denotes a value ranging from 0 to 3, preferably equal to 0, - G denotes glucose, fructose or galactose, preferably glucose;
- le degré de polymérisation, c'est-à-dire la valeur de v, pouvant aller de 1 à 15, de préférence de 1 à 4; le degré moyen de polymérisation étant plus particulièrement compris entre 1 et 2. - the degree of polymerization, that is to say the value of v, which can range from 1 to 15, preferably from 1 to 4; the average degree of polymerization being more particularly between 1 and 2.
[0077] Les liaisons glucosidiques entre les motifs sucre sont généralement de type 1 - 6 ou 1 -4, de préférence de type 1 -4. De préférence, le tensioactif alkyl(poly)glycoside est un tensioactif alkyl(poly)glucoside, c’est-à-dire un tensioactif alkyl(poly)glycoside où G est un glucose. On préfère tout particulièrement les alkyl C6/C16- (poly)glucosides 1 ,4, les alkyl C6/C12-(poly)glucosides 1 ,4, et notamment les décylglucosides, les dodécylglucosides, les hetpoglucosides, les caprylyl glucosides, les capryl glucosides et les caprylyl/capryl glucosides. The glucosidic bonds between the sugar units are generally of the 1-6 or 1-4 type, preferably of the 1-4 type. Preferably, the alkyl(poly)glycoside surfactant is an alkyl(poly)glucoside surfactant, that is to say an alkyl(poly)glycoside surfactant where G is glucose. C6/C16-(poly)glucosides 1,4 alkyl, C6/C12-(poly)glucosides 1,4, and in particular decylglucosides, dodecylglucosides, hetpoglucosides, caprylyl glucosides, capryl glucosides and caprylyl/capryl glucosides.
[0078] Selon un mode de réalisation, le tensioactif est choisi parmi les capryl/capryl glucosides. According to one embodiment, the surfactant is chosen from capryl/capryl glucosides.
[0079]Parmi les produits commerciaux, on peut citer les produits vendus par la société COGNIS sous les dénominations PLANTAREN® (600 CS/ll, 1200 et 2000) ou PLANTACARE® (818, 1200 et 2000); les produits vendus par la société SEPPIC sous les dénominations ORAMIX CG 110 et ORAMIX® NS 100; les produits vendus par la société BASF sous la dénomination LUTENSOL GD 70 ou encore les produits vendus par la société CHEM Y sous la dénomination AGI O LK. Among the commercial products, mention may be made of the products sold by the company Cognis under the names PLANTAREN® (600 CS/ll, 1200 and 2000) or PLANTACARE® (818, 1200 and 2000); the products sold by the company SEPPIC under the names ORAMIX CG 110 and ORAMIX® NS 100; the products sold by the company BASF under the name LUTENSOL GD 70 or else the products sold by the company CHEM Y under the name AGI O LK.
[0080] Le tensioactif non ionique peut en outre être choisi parmi les alkyl(poly)glycosides, préférentiellement alkyl(poly)glucosides, de HLB supérieure ou égal à 10, ou supérieur ou égale à 12, ou supérieure ou égal à14. The nonionic surfactant can also be chosen from alkyl(poly)glycosides, preferably alkyl(poly)glucosides, with an HLB greater than or equal to 10, or greater than or equal to 12, or greater than or equal to 14.
[0081] Les alkyl(poly)glycosides, préférentiellement les alkyl(poly)glucosides, peuvent en outre être combinés avec des alcools gras. Alkyl(poly)glycosides, preferably alkyl(poly)glucosides, can also be combined with fatty alcohols.
[0082] Le tensioactif non ionique peut également être choisi parmi les hétéropolymères d’alkylglycosides en C8-C10 et d’esters gras de sorbitan, préférentiellement parmi les hétéropolymères d’alkylglycosides en C8-C10 et d’esters gras en C4-C20 de sorbitan, et plus préférentiellement parmi les hétéropolymères d’alkylglycosides en C10 et d’esters gras en C18 de sorbitan. Un exemple d’un tel hétéropolymère est le Poly Suga®Mulse D9 de Colonial Chemical Inc. [0083] La quantité totale de tensioactifs non ioniques dans la composition liquide antimicrobienne est supérieure ou égale à 1 % en poids, préférentiellement supérieure ou égale à 5% en poids, plus préférentiellement supérieure ou égale à 7,5% en poids, et tout préférentiellement supérieure ou égale à 10% en poids, par rapport au poids total de ladite composition liquide antimicrobienne. The nonionic surfactant can also be chosen from heteropolymers of C8-C10 alkylglycosides and fatty esters of sorbitan, preferably from heteropolymers of C8-C10 alkylglycosides and C4-C20 fatty esters of sorbitan, and more preferably from heteropolymers of C10 alkylglycosides and of C18 fatty esters of sorbitan. An example of such a heteropolymer is Poly Suga® Mulse D9 from Colonial Chemical Inc. The total amount of nonionic surfactants in the antimicrobial liquid composition is greater than or equal to 1% by weight, preferably greater than or equal to 5% by weight, more preferably greater than or equal to 7.5% by weight, and any preferably greater than or equal to 10% by weight, relative to the total weight of said liquid antimicrobial composition.
[0084]Avantageusement, la quantité totale de tensioactifs non ioniques présente dans la composition liquide antimicrobienne peut aller de 1 % à 50% en poids, préférentiellement de 1 % à 40%, préférentiellement de 5% à 40% en poids, préférentiellement 5% à 30% en poids, plus préférentiellement de 7,5% à 30% en poids, plus préférentiellement 7,5 à 20% en poids, et tout préférentiellement de 10% à 20% en poids, par rapport au poids total de la composition liquide antimicrobienne. [0084] Advantageously, the total quantity of nonionic surfactants present in the liquid antimicrobial composition can range from 1% to 50% by weight, preferentially from 1% to 40%, preferentially from 5% to 40% by weight, preferentially 5% to 30% by weight, more preferably from 7.5% to 30% by weight, more preferably 7.5 to 20% by weight, and most preferably from 10% to 20% by weight, relative to the total weight of the composition antimicrobial liquid.
[0085] Le rapport de la masse sèche totale de tensioactifs non ioniques sur la masse sèche totale d’huiles essentielles peut en outre être supérieur ou égal à 2, préférentiellement supérieur ou égale à 3, plus préférentiellement supérieur ou égale à 4, et tout préférentiellement supérieur ou égal à 5. Le ou les tensioactifs non ioniques sont avantageusement présents dans la composition antimicrobienne en une quantité qui est en excès par rapport à la quantité de la ou des huiles essentielles. La sélection de cette situation d’excès permet de solubiliser au mieux la ou les huiles essentielles dans l’eau de la composition liquide antimicrobienne, et contribue aussi à maintenir cette solubilisation dans l’eau du produit cosmétique lorsque ladite composition liquide antimicrobienne est diluée dans ledit produit cosmétique, et notamment dans l’eau dudit produit cosmétique. The ratio of the total dry mass of nonionic surfactants to the total dry mass of essential oils may also be greater than or equal to 2, preferably greater than or equal to 3, more preferably greater than or equal to 4, and any preferably greater than or equal to 5. The nonionic surfactant(s) are advantageously present in the antimicrobial composition in an amount which is in excess relative to the amount of the essential oil(s). The selection of this excess situation makes it possible to best solubilize the essential oil or oils in the water of the antimicrobial liquid composition, and also contributes to maintaining this solubilization in the water of the cosmetic product when the said antimicrobial liquid composition is diluted in said cosmetic product, and in particular in the water of said cosmetic product.
[0086]Avantageusement, selon le mode de réalisation où le tensioactif non ionique est le caprylyl/capryl glucoside, une valeur du rapport de la masse de caprylyl/capryl glucoside sur la masse d’huile essentielle supérieure ou égale à 2, de préférence supérieure ou égale à 3, plus préférentiellement supérieure ou égale à 4, tout préférentiellement supérieure ou égale à 5, permet d’obtenir une composition liquide antimicrobienne totalement transparente et stable dans le temps à l’état concentré et à l’état dilué dans l’eau. Les formulateurs de produits cosmétiques préfèrent généralement employés des ingrédients transparents pour formuler leurs produits. Advantageously, according to the embodiment where the nonionic surfactant is caprylyl/capryl glucoside, a value of the ratio of the mass of caprylyl/capryl glucoside to the mass of essential oil greater than or equal to 2, preferably greater than or equal to 3, more preferably greater than or equal to 4, most preferably greater than or equal to 5, makes it possible to obtain a completely transparent and stable antimicrobial liquid composition over time in the concentrated state and in the diluted state in the water. Cosmetic product formulators generally prefer to employ transparent ingredients to formulate their products.
[0087]Avantageusement, la sélection des tensioactifs non ioniques selon l’invention rend la composition liquide antimicrobienne compatible avec les tensioactifs ioniques et les tensioactifs zwitterioniques. Il est donc possible d’ajouter la composition antimicrobienne à un produit cosmétique comprenant un autre type de tensioactif en gardant une bonne stabilité physique de l’état du produit cosmétique, et en gardant les effets des tensioactifs ioniques ou zwitterioniques, c’est-à-dire sans masquer ou neutraliser les effets de ces tensioactifs. [0087] Advantageously, the selection of nonionic surfactants according to the invention makes the liquid antimicrobial composition compatible with ionic surfactants and zwitterionic surfactants. It is therefore possible to add the composition antimicrobial to a cosmetic product comprising another type of surfactant while maintaining good physical stability of the state of the cosmetic product, and retaining the effects of ionic or zwitterionic surfactants, that is to say without masking or neutralizing the effects of these surfactants.
[0088]Ainsi, la composition antimicrobienne selon l’invention peut être ajoutée à des shampoings ou gels douches, qui comprennent des tensioactifs anioniques, souvent en quantité élevée, tout en conservant le pouvoir détergent des tensioactifs anioniques, et en conservant l’état monophasique liquide ou gel. La composition liquide antimicrobienne peut aussi être ajoutée à une solution colorante ou un après- shampoing, comprenant généralement des tensioactifs cationiques ou des polymères cationiques, tout en conservant la capacité de coloration et la capacité de conditionnement des cheveux. [0088] Thus, the antimicrobial composition according to the invention can be added to shampoos or shower gels, which comprise anionic surfactants, often in high quantities, while retaining the detergent power of the anionic surfactants, and retaining the monophasic state liquid or gel. The liquid antimicrobial composition can also be added to a coloring solution or hair conditioner, generally comprising cationic surfactants or cationic polymers, while retaining the coloring ability and conditioning ability of the hair.
[0089] Acides carboxyliques libres [0089] Free carboxylic acids
[0090]L’acide carboxylique libre utile à la composition antimicrobienne objet de la présente demande est choisi parmi les acides monocarboxyliques et les acides polycarboxyliques, linéaires ou branchés, préférentiellement parmi les acides monocarboxyliques, les acides dicarboxyliques, et les acides tricarboxyliques, tout préférentiellement parmi les acides monocarboxyliques et les acides dicarboxyliques. The free carboxylic acid useful for the antimicrobial composition which is the subject of the present application is chosen from monocarboxylic acids and polycarboxylic acids, linear or branched, preferentially from monocarboxylic acids, dicarboxylic acids, and tricarboxylic acids, very preferentially among monocarboxylic acids and dicarboxylic acids.
[0091] Par « libre », on entend que la fonction acide carboxylique est soit sous sa forme protonée COOH, soit sous sa forme ionisée COO- associée à un contre ion H+ ou H3O+, et cela dans des proportions dépendantes de la valeur du pH de la solution aqueuse d’acide et de la force de l’acide caractérisée par son pKa. By "free", it is meant that the carboxylic acid function is either in its protonated form COOH, or in its ionized form COO- associated with a counter ion H+ or H3O+, and this in proportions dependent on the value of the pH. of the aqueous solution of acid and the strength of the acid characterized by its pKa.
[0092] Selon un mode de réalisation, l’acide carboxylique est choisi parmi les acides monocarboxyliques dont la chaîne carbonée est constituée de 2 à 12 atomes de carbones, ou de 3 à 8 atomes de carbones. On citera l’acide gluconique (pKa=3,86), l’acide lactique, l’acide glycolique, l’acide glucuronique, l’acide maltobionique, l’acide lactobionique, l’acide malique, l’acide tartarique, l’acide mandélique, les acides gras (ou acides carboxyliques à chaîne aliphatique) possédant une chaîne carbonée de 4 à 12 atomes, de préférence les acides gras naturels comme en particulier les acides propionique, butyrique, caproïque, caprylique, caprique et laurique. Selon une variante de ce mode de réalisation, l’acide carboxylique est choisi parmi l’acide gluconique, l’acide glucuronique, l’acide maltobionique, préférentiellement l’acide carboxylique est l’acide gluconique. Selon une variante de ce mode de réalisation, l’acide monocarboxylique est la forme cyclique de l’acide gluconique, appelée gluconolactone. According to one embodiment, the carboxylic acid is chosen from monocarboxylic acids whose carbon chain consists of 2 to 12 carbon atoms, or 3 to 8 carbon atoms. These include gluconic acid (pKa=3.86), lactic acid, glycolic acid, glucuronic acid, maltobionic acid, lactobionic acid, malic acid, tartaric acid, mandelic acid, fatty acids (or aliphatic chain carboxylic acids) having a carbon chain of 4 to 12 atoms, preferably natural fatty acids such as in particular propionic, butyric, caproic, caprylic, capric and lauric acids. According to a variant of this embodiment, the carboxylic acid is chosen from gluconic acid, glucuronic acid, maltobionic acid, preferentially the carboxylic acid is gluconic acid. According to a variant of this embodiment, the monocarboxylic acid is the cyclic form of gluconic acid, called gluconolactone.
[0093] Selon un autre mode de réalisation, l’acide carboxylique est choisi parmi les acides polycarboxyliques, et de préférence parmi les acides dicarboxyliques et les acides tricarboxyliques, et tout préférentiellement parmi l’acide aspartique, l’acide adipique, l’acide malonique, l’acide pimélique, l’acide succinique, l’acide glucarique, et l’acide glutarique, et encore plus préférentiellement est l’acide succinique. According to another embodiment, the carboxylic acid is chosen from polycarboxylic acids, and preferably from dicarboxylic acids and tricarboxylic acids, and most preferably from aspartic acid, adipic acid, malonic, pimelic acid, succinic acid, glucaric acid, and glutaric acid, and even more preferably is succinic acid.
[0094] Le ou les acides carboxyliques ou acides polycarboxyliques utiles à la composition liquide antimicrobienne objet de la présente demande sont en outre caractérisés par une valeur de pKa allant de 3 à 6, préférentiellement de 4 à 6. The carboxylic acid(s) or polycarboxylic acid(s) useful for the antimicrobial liquid composition which is the subject of the present application are further characterized by a pKa value ranging from 3 to 6, preferably from 4 to 6.
[0095] La quantité totale du ou des acides carboxyliques libres présente dans la composition liquide antimicrobienne peut aller de 10% à 70% en poids sec, préférentiellement de 20% à 60% en poids sec, plus préférentiellement de 25% à 50% en poids sec, et tout préférentiellement de 27,5% à 40% en poids sec, par rapport au poids total de la composition liquide antimicrobienne. The total amount of free carboxylic acid(s) present in the liquid antimicrobial composition can range from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight. dry weight, and most preferably from 27.5% to 40% by dry weight, relative to the total weight of the antimicrobial liquid composition.
[0096] Sels d’acide carboxylique [0096] Carboxylic acid salts
[0097] Le sel d’acide carboxylique utile à la composition antimicrobienne objet de la présente demande est choisi parmi les sels d’acides monocarboxyliques ou les sels d’acides polycarboxyliques, linéaires ou branchés. Dans un sel d’acide, la fonction acide carboxylique est soit sous forme protonée COOH, soit sous forme ionisée COO- associée à un contre ion métallique M+, et cela dans des proportions dépendantes de la valeur du pH de la solution aqueuse d’acide, de la constante d’acidité pKa de l’acide libre correspondant, et de la constante dissociation du sel pKd. The carboxylic acid salt useful for the antimicrobial composition which is the subject of the present application is chosen from salts of monocarboxylic acids or salts of linear or branched polycarboxylic acids. In an acid salt, the carboxylic acid function is either in the protonated form COOH, or in the ionized form COO- associated with a metallic counter ion M+, and this in proportions dependent on the pH value of the aqueous acid solution , the acidity constant pKa of the corresponding free acid, and the dissociation constant of the salt pKd.
[0098] Le ou les sels d’acides carboxyliques est ou sont choisis parmi les sels de sodium, de magnésium, de zinc, de calcium, de potassium, de fer, de lithium, d’acide carboxylique choisi parmi les acides carboxyliques de la partie « acide carboxylique libre » de la présente demande. The carboxylic acid salt or salts is or are chosen from sodium, magnesium, zinc, calcium, potassium, iron, lithium, carboxylic acid salts chosen from the carboxylic acids of "free carboxylic acid" part of the present application.
[0099]Selon un mode de réalisation, le sel d’acide carboxylique est un sel de l’acide carboxylique libre utile à la composition objet de la présente demande. Selon une variante de ce mode de réalisation, ledit acide carboxylique est réparti en au plus 35 % en poids sec en sel dudit acide carboxylique et en au moins 65 % en poids sec en ledit acide carboxylique libre. Une telle variante est l’acide gluconique répartie à 35 % en poids sec en gluconate de sodium et à 65% en poids sec en acide gluconique libre. Avantageusement un tel mélange d’acide et de son sel, présente un pH mieux toléré par la peau et est moins irritant que le seul acide peut l’être. According to one embodiment, the carboxylic acid salt is a salt of the free carboxylic acid useful for the composition that is the subject of the present application. According to a variant of this embodiment, said carboxylic acid is distributed in at most 35% by dry weight in salt of said carboxylic acid and in at least 65% by dry weight in said free carboxylic acid. One such variant is gluconic acid distributed at 35% by dry weight as sodium gluconate and 65% by dry weight as free gluconic acid. Advantageously, such a mixture of acid and its salt has a pH that is better tolerated by the skin and is less irritating than the acid alone can be.
[0100]Selon un mode de réalisation, le ou les sels d’acide carboxylique est ou sont choisis parmi les sels de sodium, de magnésium, de zinc, de calcium, de potassium, de fer, ou de lithium de l’acide gluconique ou de l’acide succinique, et de préférence le ou les sels d’acide carboxylique sont choisis parmi le gluconate de sodium et le succinate de sodium, et tout préférentiellement le sel d’acide carboxylique est le gluconate de sodium. According to one embodiment, the carboxylic acid salt or salts is or are chosen from sodium, magnesium, zinc, calcium, potassium, iron or lithium salts of gluconic acid or succinic acid, and preferably the carboxylic acid salt or salts are chosen from sodium gluconate and sodium succinate, and most preferably the carboxylic acid salt is sodium gluconate.
[0101] La quantité totale de sels d’acide carboxylique présente dans la composition liquide antimicrobienne peut aller de 1 % à 50% en poids sec, préférentiellement de 5% à 30% en poids sec, plus préférentiellement de 10% à 20% en poids sec, et tout préférentiellement de 15% à 17,5% en poids sec, par rapport au poids total de la composition liquide antimicrobienne. The total quantity of carboxylic acid salts present in the liquid antimicrobial composition can range from 1% to 50% by dry weight, preferentially from 5% to 30% by dry weight, more preferentially from 10% to 20% by dry weight. dry weight, and most preferably from 15% to 17.5% by dry weight, relative to the total weight of the antimicrobial liquid composition.
[0102] Eau [0102] Water
[0103]L’eau présente dans la composition liquide antimicrobienne peut être une eau décarbonatée, ou une eau déminéralisée. [0103] The water present in the antimicrobial liquid composition can be decarbonated water, or demineralized water.
[0104]La quantité d’eau présente dans la composition liquide antimicrobienne peut aller de 20% à 75% en poids, préférentiellement de 30% à 65% en poids, plus préférentiellement de 35% à 55% en poids, par rapport au poids total de la composition liquide antimicrobienne. The amount of water present in the antimicrobial liquid composition can range from 20% to 75% by weight, preferably from 30% to 65% by weight, more preferably from 35% to 55% by weight, relative to the weight total antimicrobial liquid composition.
[0105]pH de la composition liquide antimicrobienne : [0105]pH of the antimicrobial liquid composition:
[0106]Le pH de la composition liquide antimicrobienne objet de la présente demande peut aller de 2 à 9, préférentiellement de 3 à 8, plus préférentiellement de 4 à 7, et encore plus préférentiellement de 4,5 à 6,5, et encore plus préférentiellement de 5,5 à 6,2. The pH of the antimicrobial liquid composition that is the subject of the present application can range from 2 to 9, preferably from 3 to 8, more preferably from 4 to 7, and even more preferably from 4.5 to 6.5, and even more more preferably from 5.5 to 6.2.
[0107] Conservateurs [0107] Preservatives
[0108] On pourra concernant les conservateurs usuels en question et leurs dosages en fonction des applications précises, se référer à la liste du règlement cosmétique N°1223/2009 en l’annexe 5 intitulé « liste des agents conservateurs admis dans les produits cosmétiques ». [0108] Concerning the usual preservatives in question and their dosages depending on the specific applications, we can refer to the list of the cosmetic regulations No. 1223/2009 in appendix 5 entitled “list of preservatives allowed in cosmetic products”.
[0109] Ainsi, le conservateur peut être choisi parmi l’acide propionique, le propionate de calcium, le formaldéhyde, le paraformaldéhyde, l’o-phenylphenol ou ses sels, le zinc pyrithione, les sulfites, bisulfites ou métabisulfites de sodium, d’ammonium, de potassium, le chlorobutanol, le méthylparaben, l’éthylparaben, le propylparaben, le butylparaben, l’acide formique et ses sels tels que le formate de sodium, l’acide benzoïque et ses sels tels que le benzoate de sodium, l’acide sorbique et ses sels , tels que le sorbate de calcium, le sorbate de sodium, le sorbate de potassium, l’acide salicylique et ses sels, l’acide déhydroacétique et ses sels tels que le déhydroacétate de sodium, l’acide undécylénique et ses sels tels que l’undécylénate de calcium, l’undécylénate de potassium, l’undécylénate de sodium, le phenoxyéthanol, le 1 ,2- Dimethylol-5,6-dimethylhydantoine, l’alcool benzylique, le chlorhexidine, le diacetate de chlorhexidine, le digluconate de chlorhexidine, le dihydrochlorure de chlorhexidine, le chlorure de behentrimonium, le chlorure de cetrimonium, le bromure de cetrimonium, le chlorure de laurtrimonium, le bromure de laurtrimonium, le chlorure de steartrimonium, le bromure de steartrimonium, l’hexamidine, le diisethionate d’hexamidine, le chlorphenesin, le chlorure de benzalkonium, le bromure de benzalkonium, le saccharinate de benzalkonium, I’ éthyl lauroyl arginate. Thus, the preservative can be chosen from propionic acid, calcium propionate, formaldehyde, paraformaldehyde, o-phenylphenol or its salts, zinc pyrithione, sodium sulphites, bisulphites or metabisulphites, d ammonium, potassium, chlorobutanol, methylparaben, ethylparaben, propylparaben, butylparaben, formic acid and its salts such as sodium formate, benzoic acid and its salts such as sodium benzoate, sorbic acid and its salts, such as calcium sorbate, sodium sorbate, potassium sorbate, salicylic acid and its salts, dehydroacetic acid and its salts such as sodium dehydroacetate, undecylenic acid and its salts such as calcium undecylenate, potassium undecylenate, sodium undecylenate, phenoxyethanol, 1,2-dimethylol-5,6-dimethylhydantoin, benzyl alcohol, chlorhexidine, diacetate chlorhexidine, chlorhexidine digluconate, dihydrochlor chlorhexidine ure, behentrimonium chloride, cetrimonium chloride, cetrimonium bromide, laurtrimonium chloride, laurtrimonium bromide, steartrimonium chloride, steartrimonium bromide, hexamidine, hexamidine diisethionate, chlorphenesin, benzalkonium chloride, benzalkonium bromide, benzalkonium saccharinate, ethyl lauroyl arginate.
[0110]Selon un mode de réalisation, la composition antimicrobienne est un activateur de conservateur pour les conservateurs suivants : acide benzoique, benzoate de sodium, acide salicylique et ses sels, acide sorbique, sorbate de calcium, sorbate de sodium, sorbate de potassium, acide déhydroacétique, déhydroacétate de sodium, acide undécylénique, undécylénate de calcium, undécylénate de potassium, undécylénate de sodium, phenoxyéthanol, 1 ,2-Dimethylol-5,6-dimethylhydantoine, alcool benzylique, chlorhexidine, diacetate de chlorhexidine, digluconate de chlorhexidine, dihydrochlorure de chlorhexidine, chlorure de behentrimonium, chlorure de cetrimonium, bromure de cetrimonium, chlorure de laurtrimonium, bromure de laurtrimonium, chlorure de steartrimonium, bromure de steartrimonium, hexamidine, diisethionate d’hexamidine, chlorphenesin, chlorure de benzalkonium, bromure de benzalkonium, saccharinate de benzalkonium, éthyl lauroyl arginate. According to one embodiment, the antimicrobial composition is a preservative activator for the following preservatives: benzoic acid, sodium benzoate, salicylic acid and its salts, sorbic acid, calcium sorbate, sodium sorbate, potassium sorbate, dehydroacetic acid, sodium dehydroacetate, undecylenic acid, calcium undecylenate, potassium undecylenate, sodium undecylenate, phenoxyethanol, 1,2-Dimethylol-5,6-dimethylhydantoin, benzyl alcohol, chlorhexidine, chlorhexidine diacetate, chlorhexidine digluconate, dihydrochloride chlorhexidine, behentrimonium chloride, cetrimonium chloride, cetrimonium bromide, laurtrimonium chloride, laurtrimonium bromide, steartrimonium chloride, steartrimonium bromide, hexamidine, hexamidine diisethionate, chlorphenesin, benzalkonium chloride, benzalkonium bromide, saccharinate benzalkonium, ethyl lauroyl arginate.
[0111]Selon un mode de réalisation, le conservateur est choisi parmi l’acide formique et ses sels, l’acide déhydroacétique et ses sels, l’acide benzoique et ses sels, l’acide sorbique et ses sels, le phénoxyéthanol, l’alcool benzylique et ses sels. Plus préférentiellement, le conservateur activé par la composition liquide antimicrobienne, est choisi parmi l’acide benzoique, l’acide sorbique, le phénoxyéthanol, l’alcool benzylique, le benzoate de sodium, le sorbate de potassium. Encore plus préférentiellement, le conservateur est choisi parmi le phénoxyéthanol, l’alcool benzylique, le benzoate de sodium et le sorbate de potassium. According to one embodiment, the preservative is chosen from formic acid and its salts, dehydroacetic acid and its salts, benzoic acid and its salts, sorbic acid and its salts, phenoxyethanol, benzyl alcohol and its salts. More preferably, the preservative activated by the liquid antimicrobial composition is chosen from benzoic acid, sorbic acid, phenoxyethanol, benzyl alcohol, sodium benzoate, potassium sorbate. Even more preferably, the preservative is chosen from phenoxyethanol, benzyl alcohol, sodium benzoate and potassium sorbate.
[0112]Selon un mode de réalisation, le conservateur activé par la composition liquide antimicrobienne, est choisi parmi l’acide sorbique et ses sels de calcium, de sodium, de potassium, de magnésium, ou de zinc, ou un mélange de ceux-ci. Encore plus préférentiellement, le conservateur est choisi parmi l’acide sorbique, le sorbate de calcium, le sorbate de sodium, le sorbate de potassium. Tout préférentiellement, le conservateur est le sorbate de potassium. According to one embodiment, the preservative activated by the liquid antimicrobial composition is chosen from sorbic acid and its calcium, sodium, potassium, magnesium or zinc salts, or a mixture of these. this. Even more preferably, the preservative is chosen from sorbic acid, calcium sorbate, sodium sorbate, potassium sorbate. Most preferably, the preservative is potassium sorbate.
[0113]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer le pouvoir conservateur du phénoxyéthanol vis-à-vis de Pseudomonas Aeruginosa, Escherichia Coli, de Staphylococcus aureus et Aspergillus brasiliensis. According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate the preservative power of phenoxyethanol against Pseudomonas Aeruginosa, Escherichia Coli, Staphylococcus aureus and Aspergillus brasiliensis.
[0114]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer le phénoxyéthanol et, combinée audit phénoxyéthanol, de réduire d’au moins deux logs le nombre d’unités formant colonies de Pseudomonas Aeruginosa, de Staphylococcus aureus, dAspergillus brasiliensis et d’ Escherichia Coli. According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate phenoxyethanol and, combined with said phenoxyethanol, to reduce by at least two logs the number of colony-forming units of Pseudomonas Aeruginosa, Staphylococcus aureus , Aspergillus brasiliensis and Escherichia Coli.
[0115] Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer le phénoxyéthanol et permet ainsi une réduction du nombre d’unités formant colonies par rapport au seul phénoxyéthanol, supérieure :According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate phenoxyethanol and thus allows a reduction in the number of colony-forming units compared to phenoxyethanol alone, greater:
- pour Pseudomonas Aeruginosa : d’au moins 2 logs à 7 jours, d’au moins 3 logs à 14 jours, - for Pseudomonas Aeruginosa: at least 2 logs at 7 days, at least 3 logs at 14 days,
- et pour Staphylococcus Aureus : d’au moins 3 logs à 7 jours, d’au moins 2 logs à 14 jours, - and for Staphylococcus Aureus: at least 3 logs at 7 days, at least 2 logs at 14 days,
- et pour Escherichia Coli : d’au moins 2 logs à 7 jours et à 14 jours, d’au moins 1 log à 28 jours,- et pour Aspergillus Brasiliensis : d’au moins 1 log à 14 jours et à 28 jours. [0116]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer le pouvoir conservateur de l’alcool benzylique vis-à-vis de Pseudomonas Aeruginosa, de Staphylococcus aureus, et Escherichia Coli. - and for Escherichia Coli: at least 2 logs at 7 days and at 14 days, at least 1 log at 28 days, - and for Aspergillus Brasiliensis: at least 1 log at 14 days and at 28 days. According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate the preservative power of benzyl alcohol against Pseudomonas Aeruginosa, Staphylococcus aureus, and Escherichia Coli.
[0117]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer l’alcool benzylique et permet ainsi une réduction du nombre d’unités formant colonies par rapport au seul alcool benzylique, supérieure :According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate benzyl alcohol and thus allows a reduction in the number of colony-forming units compared to benzyl alcohol alone, greater:
- pour Pseudomonas Aeruginosa : d’au moins 3 logs à 7 jours, d’au moins 4 logs à 14 jours, - for Pseudomonas Aeruginosa: at least 3 logs at 7 days, at least 4 logs at 14 days,
- et pour Staphylococcus Aureus : d’au moins 3 logs à 7 jours, d’au moins 2 logs à 14 jours, - and for Staphylococcus Aureus: at least 3 logs at 7 days, at least 2 logs at 14 days,
- et pour Escherichia Coli : d’au moins 1 log à 7 jours, d’au moins 3 logs à 14 jours, d’au moins 4 logs à 28 jours, - and for Escherichia Coli: at least 1 log at 7 days, at least 3 logs at 14 days, at least 4 logs at 28 days,
[0118]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer le pouvoir conservateur du benzoate de sodium vis-à-vis de Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis, et Candida albicans. According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate the preservative power of sodium benzoate against Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis, and Candida albicans.
[0119]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer le benzoate de sodium et permet ainsi une réduction du nombre d’unités formant colonies par rapport au seul benzoate de sodium, supérieure : According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate sodium benzoate and thus allows a reduction in the number of colony-forming units compared to sodium benzoate alone, greater than:
- pour Pseudomonas Aeruginosa : d’au moins 1 logs à 7 jours, d’au moins 3 logs à 14 jours, - for Pseudomonas Aeruginosa: at least 1 log at 7 days, at least 3 log at 14 days,
- et pour Staphylococcus Aureus : d’au moins 3 logs à 7 jours, d’au moins 1 log à 14 jours, - and for Staphylococcus Aureus: at least 3 logs at 7 days, at least 1 log at 14 days,
- et pour Escherichia Coli : d’au moins 3 logs à 14 jours, - and for Escherichia Coli: from at least 3 logs to 14 days,
- et pour Candida Albicans : d’au moins 1 log à 7 jours, d’au moins 2 logs à 24 jours, d’au moins 3 logs à 28 jours, - and for Candida Albicans: at least 1 log at 7 days, at least 2 logs at 24 days, at least 3 logs at 28 days,
- et pour Aspergillus Brasiliensis : d’au moins 1 log à 28 jours. - and for Aspergillus Brasiliensis: at least 1 log at 28 days.
[0120]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer le pouvoir conservateur du sorbate de potassium vis-à-vis de Pseudomonas Aeruginosa, de Staphylococcus aureus, d’Escherichia Coli, de Candida Albicans et d’ Aspergillus brasiliensis. [0121]Selon un mode de réalisation, la composition antimicrobienne selon l’invention permet d’activer le sorbate de potassium et permet ainsi une réduction du nombre d’unités formant colonies par rapport au seul sorbate de potassium, supérieure :According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate the preservative power of potassium sorbate against Pseudomonas Aeruginosa, Staphylococcus aureus, Escherichia Coli, Candida Albicans and 'Aspergillus brasiliensis. According to one embodiment, the antimicrobial composition according to the invention makes it possible to activate potassium sorbate and thus makes it possible to reduce the number of colony-forming units compared to potassium sorbate alone, greater than:
- pour Pseudomonas Aeruginosa : d’au moins 3 logs à 7 jours, d’au moins 5 logs à 14 jours et à 28 jours, - for Pseudomonas Aeruginosa: at least 3 logs at 7 days, at least 5 logs at 14 days and 28 days,
- et pour Staphylococcus Aureus : d’au moins 2 logs à 7 jours, - and for Staphylococcus Aureus: at least 2 logs at 7 days,
- et pour Escherichia Coli : d’au moins 3 logs à 7 jours, d’au moins 1 log à 14 jours,- and for Escherichia Coli: at least 3 logs at 7 days, at least 1 log at 14 days,
- et pour Candida Albicans : d’au moins 1 log à 7 jours, d’au moins 3 logs à 14 jours et à 28 jours, - and for Candida Albicans: at least 1 log at 7 days, at least 3 logs at 14 days and 28 days,
- et pour Aspergillus Brasiliensis : d’au moins 2 logs à 14 jours et à 28 jours. - and for Aspergillus Brasiliensis: at least 2 logs at 14 days and at 28 days.
[0122] L’utilisation d’une composition liquide antimicrobienne pour activer un conservateur de produit cosmétique dans un produit cosmétique, peut être faite avec :[0122] The use of an antimicrobial liquid composition to activate a cosmetic product preservative in a cosmetic product can be made with:
- une quantité de composition liquide antimicrobienne qui peut aller de au moins 0,1 % en poids brut, préférentiellement au moins 0,5% en poids brut, plus préférentiellement au moins 0,75 % en poids brut, de manière préférée au moins 1 % en poids brut, et de manière encore plus préférée au moins 1 ,5 % en poids brut,- an amount of antimicrobial liquid composition which can range from at least 0.1% by gross weight, preferably at least 0.5% by gross weight, more preferably at least 0.75% by gross weight, preferably at least 1 % by gross weight, and even more preferably at least 1.5% by gross weight,
- et une quantité de conservateur qui peut être jusqu’à 2,5 % en poids brut, préférentiellement jusqu’à 1 ,5 % en poids brut, plus préférentiellement jusqu’à 1 % en poids brut, de manière préférée jusqu’à 0,7 % en poids brut, et de manière encore plus préférée jusqu’à 0,6 % en poids brut, par rapport au poids total du produit cosmétique. - and an amount of preservative which can be up to 2.5% by gross weight, preferably up to 1.5% by gross weight, more preferably up to 1% by gross weight, preferably up to 0 7% by gross weight, and even more preferably up to 0.6% by gross weight, relative to the total weight of the cosmetic product.
[0123] L’utilisation d’une composition liquide antimicrobienne pour activer un conservateur de produit cosmétique dans un produit cosmétique, peut être faite avec :[0123] The use of an antimicrobial liquid composition to activate a cosmetic product preservative in a cosmetic product can be made with:
- une quantité de composition liquide antimicrobienne qui peut aller de 0,1 % à 5 % en poids brut, de préférence de 0,5 % à 3 % en poids brut, plus préférentiellement de 0,75 % à 2 % en poids brut, et tout préférentiellement de 1 % à 1 ,5 % en poids brut, de ladite au moins une composition liquide antimicrobienne,- an amount of antimicrobial liquid composition which can range from 0.1% to 5% by gross weight, preferably from 0.5% to 3% by gross weight, more preferably from 0.75% to 2% by gross weight, and most preferably from 1% to 1.5% by gross weight, of said at least one antimicrobial liquid composition,
- et une quantité de conservateur usuel, qui peut être de 0,1 % à 2,5 % en poids brut, de préférence de 0,2 % à 1 ,5 % en poids brut, plus préférentiellement de 0,3 % à 1 % en poids brut, et tout préférentiellement de 0,4 % à 0,7 % en poids brut, par rapport au poids total du produit cosmétique. - and an amount of usual preservative, which can be from 0.1% to 2.5% by gross weight, preferably from 0.2% to 1.5% by gross weight, more preferably from 0.3% to 1 % by gross weight, and most preferably from 0.4% to 0.7% by gross weight, relative to the total weight of the cosmetic product.
[0124] En fonction de la nature du conservateur employé, la composition antimicrobienne permet de réduire d’au moins 35%, voire d’au moins 50%, voire mieux encore d’au moins 60% la quantité de conservateur usuel employé dans les formulations cosmétiques. Ainsi il est généralement possible de ne les utiliser qu’à des taux très faibles ne dépassant pas 0,5% en poids brut, voire 0,4% en poids brut, par rapport au poids total du produit cosmétique. La stabilité microbiologique pourra être égale voire meilleure qu’avec le conservateur usuel utilisé seul et à la dose recommandée. Depending on the nature of the preservative used, the antimicrobial composition makes it possible to reduce by at least 35%, or even by at least 50%, or even better still by at least 60%, the quantity of usual preservative used in the cosmetic formulations. Thus it is generally possible to use them only at very low levels not exceeding 0.5% by gross weight, or even 0.4% by gross weight, relative to the total weight of the cosmetic product. The microbiological stability may be equal or even better than with the usual preservative used alone and at the recommended dose.
[0125]Compositions antimicrobiennes [0125]Antimicrobial compositions
[0126]Selon un mode de réalisation, la composition antimicrobienne objet de la présente demande comprend, ou est constituée de : [0126] According to one embodiment, the antimicrobial composition that is the subject of the present application comprises, or consists of:
- une huile essentielle constituée de citral et de géraniol, préférentiellement une huile de lemongrass constituée de citral et de géraniol, - an essential oil consisting of citral and geraniol, preferably a lemongrass oil consisting of citral and geraniol,
- d’un alkylglucoside porteur de chaines grasses comptant de 6 à 12 atomes de carbones, préférentiellement de caprylyl/capryl glucoside, - an alkylglucoside carrying fatty chains with 6 to 12 carbon atoms, preferably caprylyl/capryl glucoside,
- d’un acide carboxylique, préférentiellement d’acide gluconique ou d’acide succinique, tout préférentiellement d’acide gluconique, - a carboxylic acid, preferably gluconic acid or succinic acid, most preferably gluconic acid,
- d’un sel d’acide carboxylique, préférentiellement de gluconate de sodium ou de succinate de sodium, tout préférentiellement de gluconate de sodium, - a carboxylic acid salt, preferably sodium gluconate or sodium succinate, most preferably sodium gluconate,
- d’eau. - water.
[0127]Selon un mode de réalisation, la composition antimicrobienne comprend, ou est constituée de : According to one embodiment, the antimicrobial composition comprises, or consists of:
- une huile essentielle, de préférence de lemongrass comprenant au moins 50% en poids de citral et de géraniol par rapport au poids de ladite huile essentielle, à un pourcentage massique de 0,1 % à 10% en poids sec, préférentiellement de 0,5% à 7% en poids sec, plus préférentiellement de 1 % à 5% en poids sec, et tout préférentiellement de 1 ,5% à 3% en poids sec, - an essential oil, preferably lemongrass comprising at least 50% by weight of citral and geraniol relative to the weight of said essential oil, at a mass percentage of 0.1% to 10% by dry weight, preferably 0, 5% to 7% by dry weight, more preferably from 1% to 5% by dry weight, and most preferably from 1.5% to 3% by dry weight,
- de 1 % à 40% en poids sec d’un alkylglucoside porteur de chaines grasses comptant 6 à 12 atomes de carbone, de préférence de caprylyl/capryl glucoside, préférentiellement de 5% à 30% en poids sec, plus préférentiellement de 7,5% à 20% en poids sec, - from 1% to 40% by dry weight of an alkylglucoside carrying fatty chains containing 6 to 12 carbon atoms, preferably caprylyl/capryl glucoside, preferably from 5% to 30% by dry weight, more preferably 7, 5% to 20% by dry weight,
- de 10% à 70% en poids sec d’acide gluconique, d’acide succinique, de gluconate de sodium ou de succinate de sodium, préférentiellement de 20% à 60% en poids sec, plus préférentiellement de 25% à 50% en poids sec, et tout préférentiellement de 27,5% à 40% en poids sec, - from 10% to 70% by dry weight of gluconic acid, succinic acid, sodium gluconate or sodium succinate, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
- et d’eau, les pourcentages massiques étant exprimés par rapport au poids total de ladite composition antimicrobienne. - and water, the mass percentages being expressed relative to the total weight of said antimicrobial composition.
[0128] Les modes de réalisation avec les aldéhydes terpéniques, et sans aldéhydes benzéniques, présentent l’avantage d’être réputés généralement moins irritants et moins allergéniques pour la peau que les modes de réalisation avec des aldéhydes benzéniques. The embodiments with terpene aldehydes, and without benzene aldehydes, have the advantage of being generally considered to be less irritating and less allergenic for the skin than the embodiments with benzene aldehydes.
[0129]Selon un mode de réalisation, la présente invention concerne une composition liquide antimicrobienne comprenant, préférentiellement consistant en : According to one embodiment, the present invention relates to an antimicrobial liquid composition comprising, preferably consisting of:
- une huile essentielle choisie parmi les huiles essentielles de clou de girofle, de citronnelle, de géranium Bourbon, de geranium grass, de gingergrass, de laurier noble, de lemongrass, de lemongrass de l’ouest de l’Inde, de lemongrass de l’est de l’Inde, de litsée citronnée, de mélisse, de palmarose, de piment, de piment couronné, d’origan, d’arbre à thé, de thym, de schénanthe, - an essential oil chosen from the essential oils of clove, lemongrass, Bourbon geranium, geranium grass, gingergrass, noble laurel, lemongrass, West Indian lemongrass, Indian lemongrass, East Indian, Lemon Bed, Lemon Balm, Palmarose, Chilli, Crown Pepper, Oregano, Tea Tree, Thyme, Lemongrass,
- un tensioactif non ionique choisi parmi les alkyl(poly)glycosides, préférentiellement parmi les alkyl(poly)glucosides, - a nonionic surfactant chosen from alkyl(poly)glycosides, preferably from alkyl(poly)glucosides,
- un acide carboxylique libre choisi parmi l’acide gluconique, l’acide succinique,- a free carboxylic acid chosen from gluconic acid, succinic acid,
- de l’eau. - some water.
[0130]Selon un mode de réalisation, la composition liquide antimicrobienne comprend, préférentiellement consiste en : According to one embodiment, the antimicrobial liquid composition comprises, preferably consists of:
- une huile essentielle choisie parmi les huiles essentielles de citronnelle, et les huiles essentielles de lemongrass de l’ouest de l’Inde, de lemongrass de l’est de l’Inde, et préférentiellement parmi les huiles essentielles d’espèces du genre Cymbopogon,- an essential oil chosen from essential oils of citronella, and essential oils of lemongrass from western India, lemongrass from eastern India, and preferably from essential oils of species of the genus Cymbopogon ,
- un tensioactif non ionique choisi parmi les alkyl(poly)glycosides, préférentiellement parmi les alkyl(poly)glucosides, - a nonionic surfactant chosen from alkyl(poly)glycosides, preferably from alkyl(poly)glucosides,
- un acide carboxylique libre choisi parmi l’acide gluconique, l’acide succinique,- a free carboxylic acid chosen from gluconic acid, succinic acid,
- de l’eau. [0131]Selon un mode de réalisation, la composition liquide antimicrobienne comprend, préférentiellement consiste en : - some water. According to one embodiment, the antimicrobial liquid composition comprises, preferably consists of:
- de l’huile essentielle d’une des espèces du genre Cymbopogon, - essential oil of one of the species of the genus Cymbopogon,
- du caprylyl/capryl glucoside, - caprylyl/capryl glucoside,
- de l’acide gluconique, - gluconic acid,
- de l’eau. - some water.
[0132]Selon un mode de réalisation, la composition liquide antimicrobienne comprend [0132]According to one embodiment, the antimicrobial liquid composition comprises
- de l’huile essentielle d’une des espèces du genre Cymbopogon présente à un pourcentage massique allant de 0,1 % à 10% en poids sec, préférentiellement de 0,5% à 7% en poids sec, plus préférentiellement de 1 % à 5% en poids sec, et tout préférentiellement de 1 ,5% à 3% en poids sec, - essential oil of one of the species of the genus Cymbopogon present at a mass percentage ranging from 0.1% to 10% by dry weight, preferably from 0.5% to 7% by dry weight, more preferably from 1% to 5% by dry weight, and most preferably from 1.5% to 3% by dry weight,
- du caprylyl/capryl glucoside présent à un pourcentage massique allant de 1 % à 40% en poids sec, préférentiellement de 5% à 30% en poids sec, plus préférentiellement de 7,5% à 20% en poids sec, - caprylyl/capryl glucoside present at a mass percentage ranging from 1% to 40% by dry weight, preferably from 5% to 30% by dry weight, more preferably from 7.5% to 20% by dry weight,
- de l’acide gluconique libre présent à un pourcentage massique allant de 10% à 70% en poids sec, préférentiellement de 20% à 60% en poids sec, plus préférentiellement de 25% à 50% en poids sec, et tout préférentiellement de 27,5% à 40% en poids sec,- free gluconic acid present at a mass percentage ranging from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
- d’eau présente à un pourcentage massique allant de 20% à 75% en poids, préférentiellement de 30% à 65% en poids, plus préférentiellement de 35% à 55% en poids, les pourcentages massiques étant exprimés par rapport au poids total de la composition liquide antimicrobienne. - water present at a mass percentage ranging from 20% to 75% by weight, preferably from 30% to 65% by weight, more preferably from 35% to 55% by weight, the mass percentages being expressed relative to the total weight of the liquid antimicrobial composition.
[0133]Selon un mode de réalisation, la composition liquide antimicrobienne consiste en [0133]According to one embodiment, the antimicrobial liquid composition consists of
- de l’huile essentielle d’une des espèces du genre Cymbopogon présente à un pourcentage massique allant de 0,1 % à 10% en poids sec, préférentiellement de 0,5% à 7% en poids sec, plus préférentiellement de 1 % à 5% en poids sec, et tout préférentiellement de 1 ,5% à 3% en poids sec,- essential oil of one of the species of the genus Cymbopogon present at a mass percentage ranging from 0.1% to 10% by dry weight, preferably from 0.5% to 7% by dry weight, more preferably from 1% to 5% by dry weight, and most preferably from 1.5% to 3% by dry weight,
- du caprylyl/capryl glucoside présent à un pourcentage massique allant de 1 % à 40% en poids sec, préférentiellement de 5% à 30% en poids sec, et plus préférentiellement de 7,5% à 20% en poids sec,- caprylyl/capryl glucoside present at a mass percentage ranging from 1% to 40% by dry weight, preferably from 5% to 30% by dry weight, and more preferably from 7.5% to 20% by dry weight,
- de l’acide gluconique libre présente à un pourcentage massique allant de 10% à 70% en poids sec, préférentiellement de 20% à 60% en poids sec, plus préférentiellement de 25% à 50% en poids sec, et tout préférentiellement de 27,5% à 40% en poids sec,- free gluconic acid present at a mass percentage ranging from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
- d’eau présente à un pourcentage massique allant de 20% à 75% en poids, ou de- water present at a mass percentage ranging from 20% to 75% by weight, or
30% à 65% en poids, ou de 35% à 55% en poids, les pourcentages massiques étant exprimés par rapport au poids total de la composition liquide antimicrobienne, la somme des pourcentages massiques de tous les constituants étant égale à 100%. 30% to 65% by weight, or from 35% to 55% by weight, the mass percentages being expressed relative to the total weight of the antimicrobial liquid composition, the sum of the mass percentages of all the constituents being equal to 100%.
[0134]Selon un mode de réalisation, la composition liquide antimicrobienne objet de la présente demande comprend, préférentiellement consiste en :According to one embodiment, the liquid antimicrobial composition that is the subject of the present application comprises, preferably consists of:
- une huile essentielle choisie parmi les huiles essentielles de clou de girofle, de citronnelle, de géranium Bourbon, de geranium grass, de gingergrass, de laurier noble, de lemongrass, de lemongrass de l’ouest de l’Inde, de lemongrass de l’est de l’Inde, de litsée citronnée, de mélisse, de palmarose, de piment, de piment couronné, d’origan, d’arbre à thé, de thym, de schénanthe,- an essential oil chosen from the essential oils of clove, lemongrass, Bourbon geranium, geranium grass, gingergrass, noble laurel, lemongrass, West Indian lemongrass, Indian lemongrass, East Indian, Lemon Bed, Lemon Balm, Palmarose, Chilli, Crown Pepper, Oregano, Tea Tree, Thyme, Lemongrass,
- un tensioactif non ionique choisi parmi les alkyl(poly)glycosides, préférentiellement parmi les alkyl(poly)glucosides, - a nonionic surfactant chosen from alkyl(poly)glycosides, preferably from alkyl(poly)glucosides,
- un acide carboxylique libre choisi parmi l’acide gluconique, l’acide succinique,- a free carboxylic acid chosen from gluconic acid, succinic acid,
- et/ou un sel dudit acide carboxylique, choisi parmi les sels de calcium, de sodium, de potassium, de calcium, de magnésium, de zinc, - and/or a salt of said carboxylic acid, chosen from calcium, sodium, potassium, calcium, magnesium, zinc salts,
- de l’eau. - some water.
[0135]Selon un mode de réalisation, la composition liquide antimicrobienne objet comprend, préférentiellement consiste en : According to one embodiment, the object antimicrobial liquid composition comprises, preferably consists of:
- une huile essentielle choisie parmi les huiles essentielles de citronnelle, et les huiles essentielles de lemongrass de l’ouest de l’Inde, de lemongrass de l’est de l’Inde, et préférentiellement parmi les huiles essentielles d’espèces du genre Cymbopogon,- an essential oil chosen from essential oils of citronella, and essential oils of lemongrass from western India, lemongrass from eastern India, and preferably from essential oils of species of the genus Cymbopogon ,
- un tensioactif non ionique choisi parmi les alkyl(poly)glycosides, préférentiellement parmi les alkyl(poly)glucosides, - a nonionic surfactant chosen from alkyl(poly)glycosides, preferably from alkyl(poly)glucosides,
- un acide carboxylique libre choisi parmi l’acide gluconique, l’acide succinique,- a free carboxylic acid chosen from gluconic acid, succinic acid,
- et/ou un sel dudit acide carboxylique, choisi parmi les sels de calcium, de sodium, de potassium, de calcium, de magnésium, de zinc, [0136]Selon un mode de réalisation, la composition liquide antimicrobienne objet comprend, préférentiellement consiste en : - and/or a salt of said carboxylic acid, chosen from calcium, sodium, potassium, calcium, magnesium, zinc salts, According to one embodiment, the object antimicrobial liquid composition comprises, preferably consists of:
- de l’huile essentielle d’une des espèces du genre Cymbopogon, - essential oil of one of the species of the genus Cymbopogon,
- du caprylyl/capryl glucoside, - caprylyl/capryl glucoside,
- de l’acide gluconique, - gluconic acid,
- du gluconate de sodium, - sodium gluconate,
- de l’eau. - some water.
[0137]Selon un mode de réalisation, la composition liquide antimicrobienne comprend : [0137] According to one embodiment, the antimicrobial liquid composition comprises:
- de l’huile essentielle d’une des espèces du genre Cymbopogon présente à un pourcentage massique allant de 0,1 % à 10% en poids sec, préférentiellement de 0,5% à 7% en poids sec, plus préférentiellement de 1 % à 5% en poids sec, et tout préférentiellement de 1 ,5% à 3% en poids sec, - essential oil of one of the species of the genus Cymbopogon present at a mass percentage ranging from 0.1% to 10% by dry weight, preferably from 0.5% to 7% by dry weight, more preferably from 1% to 5% by dry weight, and most preferably from 1.5% to 3% by dry weight,
- du caprylyl/capryl glucoside présent à un pourcentage massique allant de 1 % à 40% en poids sec, préférentiellement de 5% à 30% en poids sec, plus préférentiellement de 7,5% à 20% en poids sec, - caprylyl/capryl glucoside present at a mass percentage ranging from 1% to 40% by dry weight, preferably from 5% to 30% by dry weight, more preferably from 7.5% to 20% by dry weight,
- de l’acide gluconique libre présente à un pourcentage massique allant de 10% à 70% en poids sec, préférentiellement de 20% à 60% en poids sec, plus préférentiellement de 25% à 50% en poids sec, et tout préférentiellement de 27,5% à 40% en poids sec,- free gluconic acid present at a mass percentage ranging from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
- du gluconate de sodium présent à un pourcentage massique allant de 1 % à 50% en poids sec, préférentiellement de 5% à 30% en poids sec, plus préférentiellement de 10% à 20% en poids sec, et tout préférentiellement de 15% à 17,5% en poids sec,- sodium gluconate present at a mass percentage ranging from 1% to 50% by dry weight, preferably from 5% to 30% by dry weight, more preferably from 10% to 20% by dry weight, and most preferably 15% at 17.5% by dry weight,
- d’eau présente à un pourcentage massique allant de 20% à 75% en poids, préférentiellement de 30% à 65% en poids, plus préférentiellement de 35% à 55% en poids, les pourcentages massiques étant exprimés par rapport au poids total de la composition liquide antimicrobienne. - water present at a mass percentage ranging from 20% to 75% by weight, preferably from 30% to 65% by weight, more preferably from 35% to 55% by weight, the mass percentages being expressed relative to the total weight of the liquid antimicrobial composition.
[0138]Selon un mode de réalisation, la composition liquide antimicrobienne consiste en : According to one embodiment, the antimicrobial liquid composition consists of:
- de l’huile essentielle d’une des espèces du genre Cymbopogon présente à un pourcentage massique allant de 0,1 % à 10% en poids sec, préférentiellement de 0,5% à 7% en poids sec, plus préférentiellement de 1 % à 5% en poids sec, et tout préférentiellement de 1 ,5% à 3% en poids sec,- essential oil of one of the species of the genus Cymbopogon present at a mass percentage ranging from 0.1% to 10% by dry weight, preferably from 0.5% to 7% by dry weight, more preferably from 1% to 5% by dry weight, and most preferably from 1.5% to 3 % dry weight,
- du caprylyl/capryl glucoside présent à un pourcentage massique allant de 1 % à 40% en poids sec, préférentiellement de 5% à 30% en poids sec, et plus préférentiellement de 7,5% à 20% en poids sec,- caprylyl/capryl glucoside present at a mass percentage ranging from 1% to 40% by dry weight, preferably from 5% to 30% by dry weight, and more preferably from 7.5% to 20% by dry weight,
- de l’acide gluconique libre présente à un pourcentage massique allant de 10% à 70% en poids sec, préférentiellement de 20% à 60% en poids sec, plus préférentiellement de 25% à 50% en poids sec, et tout préférentiellement de 27,5% à 40% en poids sec,- free gluconic acid present at a mass percentage ranging from 10% to 70% by dry weight, preferably from 20% to 60% by dry weight, more preferably from 25% to 50% by dry weight, and most preferably from 27.5% to 40% by dry weight,
- du gluconate de sodium présent à un pourcentage massique allant de 1 % à 50% en poids sec, préférentiellement de 5% à 30% en poids sec, plus préférentiellement de 10% à 20% en poids sec, et tout préférentiellement de 15% à 17,5% en poids sec,- sodium gluconate present at a mass percentage ranging from 1% to 50% by dry weight, preferably from 5% to 30% by dry weight, more preferably from 10% to 20% by dry weight, and most preferably 15% at 17.5% by dry weight,
- d’eau présente à un pourcentage massique allant de 20% à 75% en poids, ou de- water present at a mass percentage ranging from 20% to 75% by weight, or
30% à 65% en poids, ou de 35% à 55% en poids, les pourcentages massiques étant exprimés par rapport au poids total de la composition liquide antimicrobienne, la somme des pourcentages massiques de tous les constituants étant égale à 100%. 30% to 65% by weight, or from 35% to 55% by weight, the mass percentages being expressed relative to the total weight of the antimicrobial liquid composition, the sum of the mass percentages of all the constituents being equal to 100%.
[0139]Le choix des constituants de la composition liquide antimicrobienne objet de la présente demande a aussi l’avantage de lui conférer un indice de contenu d’origine naturel, noté CNO, de 100% les alkyl(poly)glucosides étant obtenus uniquement à partir de ressources végétales. The choice of the constituents of the antimicrobial liquid composition which is the subject of the present application also has the advantage of giving it a content index of natural origin, denoted CNO, of 100%, the alkyl(poly)glucosides being obtained only from from plant resources.
[0140]Structure de la composition antimicrobienne [0140]Structure of the antimicrobial composition
[0141]La composition antimicrobienne objet de la présente demande est sous la forme d’un liquide, qui est une dispersion d’une phase huileuse dans une phase aqueuse. Cette dispersion peut être soit une émulsion huile-dans-eau, soit une microémulsion huile-dans-eau, soit une nanoémulsion huile-dans-eau, soit une solution micellaire, selon la nature et les quantités des constituants de la composition et son procédé de production. Selon un mode de réalisation, la composition antimicrobienne est une émulsion huile-dans-eau, et présente des tailles de gouttelettes de phase huileuse allant de 0,3 micromètres à 10 micromètres. Selon un autre mode de réalisation, la composition antimicrobienne est une microémulsion huile-dans-eau ou une composition micellaire huile-dans-eau, et présente des tailles de gouttelettes allant de 0,001 micromètres à 0,3 micromètres. Les petites tailles des gouttelettes, ou des microgouttelettes ou micelles, de la composition liquide antimicrobienne la rendent opalescente ou transparente. De plus, elles contribuent aussi à améliorer la stabilité de l’huile dans l’eau, et à améliorer son activité antimicrobienne et son efficacité en tant qu’activateur de conservateur. The antimicrobial composition that is the subject of the present application is in the form of a liquid, which is a dispersion of an oily phase in an aqueous phase. This dispersion can be either an oil-in-water emulsion, or an oil-in-water microemulsion, or an oil-in-water nanoemulsion, or a micellar solution, depending on the nature and the amounts of the constituents of the composition and its process. of production. According to one embodiment, the antimicrobial composition is an oil-in-water emulsion, and has oil phase droplet sizes ranging from 0.3 micrometers to 10 micrometers. According to another embodiment, the antimicrobial composition is an oil-in-water microemulsion or an oil-in-water micellar composition, and has droplet sizes ranging from 0.001 micrometers to 0.3 micrometers. Smaller droplet sizes, or microdroplets, or micelles, of the antimicrobial liquid composition make it opalescent or transparent. In addition, they also contribute to improving the stability of the oil in water, and to improving its antimicrobial activity and its effectiveness as a preservative activator.
[0142]Selon un mode de réalisation, la phase dispersée huileuse comprend l’huile essentielle ; la phase aqueuse comprend l’acide carboxylique et/ou le sel d’acide carboxylique ; et le tensioactif est situé à l’interface entre les deux phases. La phase huileuse peut comprendre une huile « non essentielle », comme des triglycérides, afin de d’ajuster la concentration en huile essentielle dans la phase huileuse, et aussi pour réduire le potentiel caractère allergène de l’huile essentielle. La phase huileuse peut comprendre aussi des huiles comme les esters méthyliques d’huiles végétales, ou des triglycérides d’acides gras courts. La phase huileuse et la phase aqueuse peuvent aussi comprendre des additifs sans activité antimicrobienne tels que les agents de rhéologie, les colorants solubles, les pigments, les parfums, les humectants, les agents de charge. According to one embodiment, the oily dispersed phase comprises the essential oil; the aqueous phase comprises the carboxylic acid and/or the carboxylic acid salt; and the surfactant is located at the interface between the two phases. The oily phase may include a "non-essential" oil, such as triglycerides, in order to adjust the concentration of essential oil in the oily phase, and also to reduce the potential allergenicity of the essential oil. The oily phase can also include oils such as methyl esters of vegetable oils, or triglycerides of short fatty acids. The oily phase and the aqueous phase can also comprise additives without antimicrobial activity such as rheology agents, soluble dyes, pigments, perfumes, humectants, bulking agents.
[0143] Selon un autre mode de réalisation, la phase dispersée huileuse est constituée de l’huile essentielle ; la phase aqueuse est constituée d’eau, d’acide carboxylique libre et/ou de sel d’acide carboxylique ; et le tensioactif non ionique est réparti entre les deux phases. Dans ce mode de réalisation, la phase aqueuse contient comme seul et unique solvant l’eau, et est donc exempte de tout autre solvant, notamment de tout solvant organique. According to another embodiment, the oily dispersed phase consists of the essential oil; the aqueous phase consists of water, free carboxylic acid and/or carboxylic acid salt; and the nonionic surfactant is distributed between the two phases. In this embodiment, the aqueous phase contains water as the sole and unique solvent, and is therefore free of any other solvent, in particular of any organic solvent.
[0144] Avantageusement, la transparence de la composition liquide antimicrobienne et la compatibilité avec les tensioactifs ioniques permettent l’ajout de cette composition antimicrobienne dans des produits cosmétiques eux-mêmes transparents, tels que les eaux micellaires ou les gels, en conservant la transparence. Advantageously, the transparency of the antimicrobial liquid composition and the compatibility with ionic surfactants allow this antimicrobial composition to be added to cosmetic products that are themselves transparent, such as micellar waters or gels, while retaining the transparency.
[0145]En effet, la composition liquide antimicrobienne se présente sous la forme d’un liquide macroscopiquement homogène, ce qui en permet une utilisation aisée lors de la production des produits cosmétiques. La manipulation d’un liquide nécessite moins d’équipements de protection individuels ou collectifs que la manipulation d’une poudre pulvérulente. Le transfert entre contenant et le dosage précis sont aussi beaucoup plus simples et fiables que pour une poudre pulvérulente. [0146]Ainsi, la composition liquide antimicrobienne, peut-être aisément incorporée dans un produit cosmétique afin d’activer le conservateur présent, sans déstabiliser le produit cosmétique. Cette composition selon l’invention offre une bonne stabilité et comptabilité avec les produits cosmétiques, en permettant une transparence sans problème de cristallisation ou de précipitation. [0145] Indeed, the antimicrobial liquid composition is in the form of a macroscopically homogeneous liquid, which allows easy use during the production of cosmetic products. Handling a liquid requires less personal or collective protective equipment than handling a pulverulent powder. The transfer between container and the precise dosage are also much simpler and more reliable than for a pulverulent powder. [0146] Thus, the antimicrobial liquid composition can easily be incorporated into a cosmetic product in order to activate the preservative present, without destabilizing the cosmetic product. This composition according to the invention offers good stability and compatibility with cosmetic products, allowing transparency without problem of crystallization or precipitation.
[0147] Produit cosmétique [0147] Cosmetic product
[0148] La présente demande concerne également un produit cosmétique contenant comme activateur de conservateur, une composition liquide antimicrobienne selon l’invention, et au moins un conservateur usuel de produit cosmétique tel que précédemment décrit. The present application also relates to a cosmetic product containing, as a preservative activator, an antimicrobial liquid composition according to the invention, and at least one usual cosmetic product preservative as described above.
[0149]Selon un mode de réalisation, le produit cosmétique comprend : [0149]According to one embodiment, the cosmetic product comprises:
- jusqu’à 2,5 % en poids brut, préférentiellement jusqu’à 1 ,5 % en poids brut, plus préférentiellement jusqu’à 1 % en poids brut, de manière préférée jusqu’à 0,7 % en poids brut, et de manière encore plus préférée jusqu’à 0,6 % en poids brut, dudit au moins un conservateur, - up to 2.5% by gross weight, preferably up to 1.5% by gross weight, more preferably up to 1% by gross weight, preferably up to 0.7% by gross weight, and even more preferably up to 0.6% by gross weight, of said at least one preservative,
- et au moins 0,1 % en poids brut, préférentiellement au moins 0,5% en poids brut, plus préférentiellement au moins 0,75 % en poids brut, de manière préférée au moins 1 % en poids brut, et de manière encore plus préférée au moins 1 ,5 % en poids brut, de ladite au moins une composition liquide antimicrobienne, par rapport au poids total du produit cosmétique. - and at least 0.1% by gross weight, preferably at least 0.5% by gross weight, more preferably at least 0.75% by gross weight, preferably at least 1% by gross weight, and even more more preferably at least 1.5% by gross weight, of said at least one antimicrobial liquid composition, relative to the total weight of the cosmetic product.
[0150] De préférence, le produit cosmétique comprend : [0150] Preferably, the cosmetic product comprises:
-jusqu’à 0,5 % en poids brut, de préférence jusqu’à 0,4 % en poids brut dudit au moins un conservateur, -up to 0.5% by gross weight, preferably up to 0.4% by gross weight of said at least one preservative,
- et au moins 2,0 % en poids brut, préférentiellement au moins 3 % en poids brut, de ladite au moins une composition liquide antimicrobienne, par rapport au poids total du produit cosmétique. - and at least 2.0% by gross weight, preferably at least 3% by gross weight, of said at least one antimicrobial liquid composition, relative to the total weight of the cosmetic product.
[0151]Tout préférentiellement, le produit cosmétique comprend : [0151] Most preferably, the cosmetic product comprises:
- de 0,1 % à 2,5 % en poids brut, de préférence de 0,2 % à 1 ,5 % en poids brut, plus préférentiellement de 0,3 % à 1 % en poids brut, et tout préférentiellement de 0,4 % à 0,7 % en poids brut, dudit au moins un conservateur, - et de 0,1 % à 5 % en poids brut, de préférence de 0,5 % à 3 % en poids brut, plus préférentiellement de 0,75 % à 2 % en poids, brut et tout préférentiellement de 1 % à 1 ,5 % en poids brut, de ladite au moins une composition liquide antimicrobienne, par rapport au poids total du produit cosmétique. - from 0.1% to 2.5% by gross weight, preferably from 0.2% to 1.5% by gross weight, more preferably from 0.3% to 1% by gross weight, and most preferably from 0 4% to 0.7% by gross weight, of said at least one preservative, - and from 0.1% to 5% by gross weight, preferably from 0.5% to 3% by gross weight, more preferably from 0.75% to 2% by weight, gross and most preferably from 1% to 1 5% by gross weight, of said at least one antimicrobial liquid composition, relative to the total weight of the cosmetic product.
[0152]Selon un mode de réalisation, le produit cosmétique comprend une seule et unique composition liquide antimicrobienne selon la présente demande, et un seul et unique conservateur. According to one embodiment, the cosmetic product comprises a single and single antimicrobial liquid composition according to the present application, and a single and single preservative.
[0153] Le produit cosmétique peut se présenter sous toutes les formes ou états physiques connus, à savoir être une émulsion huile-dans-eau, une émulsion eau-dans- huile, une suspension, une mousse, une solution vraie, une solution micellaire, une solution hydroalcoolique, une pâte, un gel, une poudre, un comprimé, une lingette. De préférence, le produit se présente sous une forme choisie parmi une émulsion huile- dans-eau, une émulsion eau-dans-huile, une suspension, une mousse, une solution vraie, une solution micellaire, une solution hydroalcoolique, une pâte, un gel. Tout préférentiellement, le produit se présente sous une forme choisie parmi une émulsion huile-dans-eau, une émulsion eau-dans-huile, une suspension, une mousse, une solution vraie, une solution micellaire, une pâte, un gel. The cosmetic product can be in any known form or physical state, namely an oil-in-water emulsion, a water-in-oil emulsion, a suspension, a foam, a true solution, a micellar solution , a hydroalcoholic solution, a paste, a gel, a powder, a tablet, a wipe. Preferably, the product is in a form chosen from an oil-in-water emulsion, a water-in-oil emulsion, a suspension, a foam, a true solution, a micellar solution, a hydroalcoholic solution, a paste, a freeze. Most preferably, the product is in a form chosen from an oil-in-water emulsion, a water-in-oil emulsion, a suspension, a foam, a true solution, a micellar solution, a paste, a gel.
[0154] Le produit cosmétique du fait de la neutralité de la composition selon l’invention et de sa haute compatibilité avec la très grande majorité des huiles et corps gras, alcools, surfactants, émulsionnants, solubilisants, conditionneurs, agents filmogènes, épaississants, gélifiants, agents de neutralisation, voire aussi des actifs, peut être formulé sans difficulté particulière et de façon très large avec les ingrédients habituellement retenus. The cosmetic product due to the neutrality of the composition according to the invention and its high compatibility with the vast majority of oils and fatty substances, alcohols, surfactants, emulsifiers, solubilizers, conditioners, film-forming agents, thickeners, gelling agents , neutralizing agents, or even active agents, can be formulated without particular difficulty and in a very broad manner with the ingredients usually selected.
[0155]Procédé de préparation d’une composition liquide antimicrobienne selon l’invention [0155] Process for preparing a liquid antimicrobial composition according to the invention
[0156]Le protocole suivant décrit la préparation d’une composition antimicrobienne constituée d’huile(s) essentielle(s), d’acide gluconique, de gluconate de sodium et d’un tensioactif solubilisant. Lorsque le tensioactif solubilisant est sous la forme d’une poudre, on le dissout dans une quantité d’eau minimale. Dans un bêcher ouvert, on ajoute lentement la quantité requise d’huile(s) essentielle(s) à la quantité requise de solution de tensioactif solubilisant, sous agitation douce (par exemple 500-1000 rpm au moteur Rayneri équipé d’une hélice) et à température ambiante (22°C), jusqu’à obtenir une solution homogène. On ajoute cette solution aqueuse d’huile(s) essentielle(s) et de solubilisant à une solution aqueuse d’acide gluconique composée de la quantité requise d’acide gluconique libre et de gluconate de sodium, sous agitation douce (par exemple 500-1000 rpm au moteur Rayneri équipé d’une hélice) et à température ambiante (22°C), jusqu’à obtenir une solution homogène. The following protocol describes the preparation of an antimicrobial composition consisting of essential oil(s), gluconic acid, sodium gluconate and a solubilizing surfactant. When the solubilizing surfactant is in the form of a powder, it is dissolved in a minimum quantity of water. In an open beaker, slowly add the required amount of essential oil(s) to the required amount of solubilizing surfactant solution, with gentle stirring (eg 500-1000 rpm using a Rayneri motor equipped with a propeller). and at room temperature (22°C), up to obtain a homogeneous solution. This aqueous solution of essential oil(s) and solubilizer is added to an aqueous solution of gluconic acid composed of the required quantity of free gluconic acid and sodium gluconate, with gentle stirring (for example 500- 1000 rpm using a Rayneri motor fitted with a propeller) and at ambient temperature (22° C.), until a homogeneous solution is obtained.
[0157] Utilisée en tant qu’activateur de conservateur, la composition antimicrobienne peut être ajoutée au produit cosmétique en fin de préparation, autrement dit après que celui-ci ait été préparé, quand la préparation dudit produit cosmétique comporte des étapes de chauffage à haute température 60-80°C sur des durées dépassant quelques minutes. Lorsque la préparation du produit cosmétique est faite intégralement à température ambiante, la composition antimicrobienne peut être ajoutée dès les premières étapes de préparation, mais il est préférable de l’ajouter en fin de préparation du produit cosmétique. [0157] Used as a preservative activator, the antimicrobial composition can be added to the cosmetic product at the end of preparation, in other words after the latter has been prepared, when the preparation of said cosmetic product includes high-temperature heating steps. temperature 60-80°C for periods exceeding a few minutes. When the preparation of the cosmetic product is carried out entirely at room temperature, the antimicrobial composition can be added from the first stages of preparation, but it is preferable to add it at the end of the preparation of the cosmetic product.
[0158]Autres applications possibles : [0158] Other possible applications:
[0159]La composition antimicrobienne selon l’invention peut également trouver des usages hors cosmétiques et peut notamment convenir à stabiliser microbiologiquement des compositions pharmaceutiques, alimentaires ou industrielles comme par exemple des compositions liquides détergentes, des compositions liquide de lavage, des colles amylacées. The antimicrobial composition according to the invention can also find non-cosmetic uses and can in particular be suitable for microbiologically stabilizing pharmaceutical, food or industrial compositions such as, for example, liquid detergent compositions, liquid washing compositions, starch adhesives.
[0160] Un autre objet de la présente demande est l’utilisation d’une composition antimicrobienne selon la présente demande pour tuer les microorganismes, ou les microorganismes pathogènes, ou inhiber la croissance des microorganismes ou des microorganismes pathogènes, sur ou dans un substrat non vivant ou artificiel. Une telle application concerne par exemple la désinfection des surfaces (les sols, les murs, les portes, les poignées de portes), désinfection/conservation de produits liquides industriels tels que les solutions aqueuses d’amidons, de protéine, ou de fibre. Another object of the present application is the use of an antimicrobial composition according to the present application for killing microorganisms, or pathogenic microorganisms, or inhibiting the growth of microorganisms or pathogenic microorganisms, on or in a substrate not living or artificial. Such an application concerns, for example, the disinfection of surfaces (floors, walls, doors, door handles), disinfection/conservation of industrial liquid products such as aqueous solutions of starches, proteins, or fibers.
Exemples Examples
[0161] Exemple 1 : sélection d’un tensioactif solubilisant pour atteindre les critères de transparence [0161] Example 1: selection of a solubilizing surfactant to achieve the transparency criteria
[0162]Cet exemple présente la sélection d’un tensioactif solubilisant et du rapport de la masse brute de tensioactif sur la masse brute d’huile essentielle, pour obtenir une solution aqueuse d’huile essentielle de lemongrass Cymbopogon flexuosus qui soit transparente aussi bien à l’état concentré qu’à l’état diluée dans de l’eau. Un tensioactif solubilisant sera acceptable si les deux critères de transparence sont satisfaits. Seuls les principaux tensioactifs testés ayant donné des résultats sont présentés ici. Le rapport de la masse brute de tensioactif sur la masse brute d’huile essentielle est noté « rapport brut TA/HE » ci-après. This example presents the selection of a solubilizing surfactant and the ratio of the gross mass of surfactant to the gross mass of essential oil, to obtain a aqueous solution of essential oil of lemongrass Cymbopogon flexuosus which is transparent both in the concentrated state and in the state diluted in water. A solubilizing surfactant will be acceptable if both transparency criteria are met. Only the main surfactants tested which gave results are presented here. The ratio of the gross mass of surfactant to the gross mass of essential oil is denoted “raw TA/HE ratio” below.
[0163] Pour chaque tensioactif solubilisant à tester (tableau 1 ), on prépare une composition liquide avec les masses de constituants suivantes : - 1 ,2 grammes d’acide gluconique (sous forme sèche), For each solubilizing surfactant to be tested (Table 1), a liquid composition is prepared with the following masses of constituents: - 1.2 grams of gluconic acid (in dry form),
- 3 grammes d’eau déminéralisée, - 3 grams of demineralised water,
- 2,4 grammes d’huile essentielle de lemongrass « Cymbopogon flexuosus Oil® » du fournisseur Elixens, - 2.4 grams of lemongrass essential oil "Cymbopogon flexuosus Oil®" from the supplier Elixens,
- 14,4 ou 19,2 ou 24 grammes bruts, c’est-à-dire grammes de produit sous sa forme disponible dans le commerce, d’un tensioactif solubilisant du tableau 1 (tous étant des tensioactifs non ioniques) pour atteindre un rapport brut TA/HE, respectivement, de 6, 8 ou 10. - 14.4 or 19.2 or 24 gross grams, i.e. grams of product in its commercially available form, of a solubilizing surfactant from Table 1 (all being nonionic surfactants) to achieve a crude TA/HE ratio, respectively, of 6, 8 or 10.
[0164] Le protocole de préparation d’une composition liquide est le suivant : The protocol for preparing a liquid composition is as follows:
- on prépare un premier pré-mélange en dissolvant l’acide gluconique dans la masse d’eau sous agitation douce à 20-22°C, - a first premix is prepared by dissolving the gluconic acid in the mass of water with gentle stirring at 20-22°C,
- on prépare un second pré-mélange en ajoutant à la masse d’huile essentielle, la masse requise de tensioactif solubilisant, et on agite pour permettre à l’huile essentielle d’être bien dispersée et obtenir un liquide homogène, - a second premix is prepared by adding to the mass of essential oil, the required mass of solubilizing surfactant, and stirring to allow the essential oil to be well dispersed and to obtain a homogeneous liquid,
- on ajoute ensuite le second pré-mélange dans le premier pré-mélange, et on maintient sous agitation douce non-cisaillante pendant environ 20 minutes, pour laisser le temps au pré-mélange de tensioactif et d’huile essentielle de se disperser, et ainsi à la composition liquide de se stabiliser. - the second pre-mixture is then added to the first pre-mixture, and the mixture is maintained under gentle non-shearing agitation for about 20 minutes, to allow time for the pre-mixture of surfactant and essential oil to disperse, and thus the liquid composition to stabilize.
[0165] Immédiatement après la préparation, on observe à l’œil nu l’état de la composition liquide préparée afin d’évaluer sa transparence et son homogénéité, notamment sur toute la hauteur de l’échantillon, et afin de rechercher l’éventuelle présence de plusieurs phases ou de particules solides (qui se seraient formées par précipitation instantanément, ou par cristallisation plus lente). On désigne cet état par « composition liquide concentrée ». Sur une moitié du volume de composition liquide, on poursuit ces observations durant un stockage à température de 20-22°C durant 1 mois. Immediately after the preparation, the state of the liquid composition prepared is observed with the naked eye in order to evaluate its transparency and its homogeneity, in particular over the entire height of the sample, and in order to search for the possible presence of several phases or solid particles (which would have formed by instantaneous precipitation, or by slower crystallization). This state is denoted by “concentrated liquid composition”. On half of the volume of liquid composition, these observations are continued during storage at a temperature of 20-22° C. for 1 month.
[0166]Sur l’autre moitié, on réalise un test de comportement à la dilution dans l’eau. On dilue 1 ,5 grammes de la composition liquide dans une masse d’eau de 98,5 grammes. On observe à l’œil nu l’état de l’eau additionnée de la composition liquide, afin d’évaluer sa transparence et son homogénéité, notamment sur toute la hauteur de l’échantillon, et de rechercher l’éventuelle présence de plusieurs phases ou de particules solides. C’est l’état « après dilution dans l’eau ». On poursuit ces observations durant un stockage à température de 20-22°C durant 1 mois. On the other half, a test of behavior on dilution in water is carried out. 1.5 grams of the liquid composition are diluted in a mass of water of 98.5 grams. The state of the water to which the liquid composition has been added is observed with the naked eye, in order to assess its transparency and its homogeneity, in particular over the entire height of the sample, and to search for the possible presence of several phases. or solid particles. This is the state "after dilution in water". These observations are continued during storage at a temperature of 20-22° C. for 1 month.
[0167] Pour l’état de « composition concentrée » et pour l’état « après dilution dans l’eau », la transparence et l’homogénéité sont qualifiées et évaluées comme suit :For the state of "concentrated composition" and for the state "after dilution in water", the transparency and the homogeneity are qualified and evaluated as follows:
- « échec » : présence de particules solides, notamment au fond de l’échantillon ; ou présence d’au moins 2 phases, dont généralement une surnageante ; présence d’une pâte, notamment au fond de l’échantillon ; turbidité légère à forte, visible à l’œil nu ; transparence hétérogène, avec une partie supérieure et une partie inférieure visiblement différentes ; aspect crémeux, notamment ivoire.- “failure”: presence of solid particles, in particular at the bottom of the sample; or presence of at least 2 phases, generally including a supernatant; presence of paste, particularly at the bottom of the sample; slight to strong turbidity, visible to the naked eye; heterogeneous transparency, with a visibly different upper and lower part; creamy appearance, notably ivory.
- « réussite » : opalescence quasiment imperceptible ; transparence homogène et quasiment parfaite à l’œil nu ; aucune turbidité visible à l’œil nu. - “success”: almost imperceptible opalescence; homogeneous and almost perfect transparency to the naked eye; no turbidity visible to the naked eye.
[0168] Les résultats de transparence et d’homogénéité de la « composition liquide concentrée » sont présentés dans le tableau 2, et les résultats de transparence et d’homogénéité « après dilution dans l’eau » sont présentés dans le tableau 3. The results of transparency and homogeneity of the "concentrated liquid composition" are presented in table 2, and the results of transparency and homogeneity "after dilution in water" are presented in table 3.
[0169] [Tableau 1 ] [0169] [Table 1 ]
[0171][Tableau 3] [0171][Table 3]
[0172] Les tensioactifs A, E et F permettent de fournir une composition liquide concentrée qui soit transparente. The surfactants A, E and F make it possible to provide a concentrated liquid composition which is transparent.
[0173] Les tensioactifs B, C et G échouent à fournir une composition liquide concentrée qui soit transparente, mais permettent la transparence après dilution dans l’eau. Le tensioactif F permet d’obtenir la transparence après dilution dans l’eau. [0173] Surfactants B, C and G fail to provide a concentrated liquid composition which is transparent, but allow transparency after dilution in water. Surfactant F provides transparency after dilution in water.
[0174]Ainsi, les tensioactifs A, B, C, E, F et G peuvent convenir à la composition liquide antimicrobienne objet de la présente demande. Thus, the surfactants A, B, C, E, F and G may be suitable for the liquid antimicrobial composition which is the subject of the present application.
[0175] Parmi tous les tests réalisés, seul le tensioactif solubilisant F, c’est-à-dire le caprylyl/capryl glucoside, permet de satisfaire à la fois le critère de transparence et d’homogénéité de la composition liquide concentrée, et le même critère après dilution dans l’eau, et cela pour des valeurs du rapport brut TA/HE allant de 8 à 10. Dans le cas du tensioactif non ionique solubilisant caprylyl/capryl glucoside, les valeurs du rapport brut TA/HE allant de 8 à 10 équivalent à des valeurs d’un rapport de la masse sèche de tensioactif sur la masse sèche d’huile essentielle allant de 4 à 5 (car ce tensioactif comprend 50% d’eau et 50% caprylyl/capryl glucoside sec). Among all the tests carried out, only the solubilizing surfactant F, that is to say caprylyl/capryl glucoside, makes it possible to satisfy both the criterion of transparency and homogeneity of the concentrated liquid composition, and the same criterion after dilution in water, and this for values of the crude TA/HE ratio ranging from 8 to 10. In the case of the nonionic surfactant solubilizing caprylyl/capryl glucoside, the values of the crude TA/HE ratio ranging from 8 to 10 are equivalent to values of a ratio of the dry mass of surfactant to the dry mass of essential oil ranging from 4 to 5 (because this surfactant comprises 50% water and 50% caprylyl/dry capryl glucoside).
[0176] Exemple 2 : préparations de compositions antimicrobiennes Example 2: preparations of antimicrobial compositions
[0177] Les ingrédients utilisés sont présentés dans le tableau 4. Les compositions des compositions antimicrobiennes objet de la présente demande sont présentées dans le tableau 5. The ingredients used are shown in Table 4. The compositions of the antimicrobial compositions that are the subject of the present application are shown in Table 5.
[0178] [Tableau 4] [0178] [Table 4]
0179] [Tableau 5] 0179] [Table 5]
[0180]Les compositions antimicrobiennes 40 et 43 sont préparées selon le protocole suivant : The antimicrobial compositions 40 and 43 are prepared according to the following protocol:
[0181] Dans un bêcher ouvert, on ajoute lentement la quantité requise d’huile essentielle à la quantité requise de solution de tensioactif solubilisant, sous agitation douce, par exemple 500-1000 rpm au moteur Rayneri équipé d’une hélice, et à température ambiante de 22°C, jusqu’à obtenir une solution homogène. On ajoute cette solution aqueuse d’huile essentielle et de solubilisant à une solution aqueuse d’acide gluconique et de gluconate de sodium. In an open beaker, the required quantity of essential oil is slowly added to the required quantity of solubilizing surfactant solution, with gentle stirring, for example 500-1000 rpm using a Rayneri motor equipped with a propeller, and at temperature room temperature of 22°C, until a homogeneous solution is obtained. This aqueous solution of essential oil and solubilizer is added to an aqueous solution of gluconic acid and sodium gluconate.
[0182] Exemple 3 : mise en évidence des propriétés de stabilisation microbioloqiquesExample 3: Demonstration of Microbiological Stabilization Properties
[0183] Les activités antibactériennes et antifongiques des compositions préparées à l’exemple 2 sont démontrées au travers de tests de croissance in-vitro sur des milieux de culture standards pour les micro-organismes suivants : Escherichia coli ATCC® 8739, Pseudomonas Aeruginosa ATCC® 9027, Staphylococcus Aureus ATCC® 6538, Candida Albicans ATCC® 10231 , et Aspergillus Brasiliensis ATCC® 16404. Ces tests comportent des comparatifs avec les constituants des compositions pris isolément, et pris en combinaison de deux constituants, afin d’identifier les synergies d’activité antimicrobienne sur ces microorganismes. [0184] Pour chaque micro-organisme, on prépare autant de tubes à essai que de produits à tester, c’est-à-dire la composition antimicrobienne, les constituants seuls, ou les combinaisons de deux constituants, ainsi qu’un témoin, avec le milieu de culture adapté au micro-organisme : « bouillon dextrose à la pomme de terre » pour Aspergillus Brasiliensis ; « Yeast Molds » pour Candida Albicans ; « bouillon tryptone soja » pour Escherichia Coli ; « milieu » pour Staphylococcus Aureus ; et « milieu » pour Pseudomonas Aeruginosa. On ajoute ensuite dans chaque tube à essai une dose de produit à tester selon le tableau 6 ci-dessous, exprimée en pourcentage poids/volume. Par exemple, un pourcentage de 1 ,5 % poids/volume signifie que pour 100 mL de milieu de culture, on ajoute 1 ,5 g de produit à tester. Puis on homogénéise soigneusement par aspirations-refoulements. The antibacterial and antifungal activities of the compositions prepared in Example 2 are demonstrated through in vitro growth tests on standard culture media for the following microorganisms: Escherichia coli ATCC® 8739, Pseudomonas Aeruginosa ATCC® 9027, Staphylococcus Aureus ATCC® 6538, Candida Albicans ATCC® 10231, and Aspergillus Brasiliensis ATCC® 16404. These tests include comparisons with the constituents of the compositions taken in isolation, and taken in combination of two constituents, in order to identify the synergies of antimicrobial activity on these microorganisms. For each microorganism, as many test tubes are prepared as there are products to be tested, that is to say the antimicrobial composition, the constituents alone, or the combinations of two constituents, as well as a control, with the culture medium adapted to the microorganism: “potato dextrose broth” for Aspergillus Brasiliensis; “Yeast Molds” for Candida Albicans; "tryptone soy broth" for Escherichia Coli; "medium" for Staphylococcus Aureus; and "middle" for Pseudomonas Aeruginosa. A dose of product to be tested according to Table 6 below, expressed as a weight/volume percentage, is then added to each test tube. For example, a percentage of 1.5% weight/volume means that for 100 mL of culture medium, 1.5 g of product to be tested are added. Then we homogenize carefully by suction-repression.
[0185] [Tableau 6] [0186] Chaque tube à essai est inoculé avec une quantité connue de microorganismes : 10A3 unités formant colonies par millilitre de gélose (noté ufc/mL) pour Aspergillus brasiliensis ; 10A4 ufc/mL pour les Escherichia coli et Candida Albicans ; 10A5 ufc/mL pour Staphylococcus aureus et Pseudomonas aeruginosa. A l’issue de l’inoculation, les milieux inoculés sont à nouveau soigneusement homogénéisés par aspirations-refoulements. [0185] [Table 6] Each test tube is inoculated with a known quantity of microorganisms : 10 to 3 colony-forming units per milliliter of agar (denoted cfu/mL) for Aspergillus brasiliensis; 10 A 4 cfu/mL for Escherichia coli and Candida Albicans; 10 to 5 cfu /mL for Staphylococcus aureus and Pseudomonas aeruginosa. At the end of the inoculation, the inoculated media are again carefully homogenized by aspiration-discharge.
[0187] Les échantillons inoculés avec Aspergillus brasiliensis sont incubés à 30°C (+/- 2,5°C) pendant 48 heures. Les échantillons inoculés avec les autres souches sont incubés à 37°C (+/-2,5°C) pendant 48 heures. The samples inoculated with Aspergillus brasiliensis are incubated at 30° C. (+/- 2.5° C.) for 48 hours. The samples inoculated with the other strains are incubated at 37°C (+/-2.5°C) for 48 hours.
[0188] Des prélèvements et dénombrements des microorganismes sont effectués à 30 minutes, 24 heures et 48 heures pour chaque micro-organisme. Les échantillons inoculés sont prélevés, dilués en série dans du diluant (Peptone de caséine 1 g/L, chlorure de sodium 8.5g/L, pH 7) et déposés respectivement sur des géloses à la pomme de terre et au dextrose pour Aspergillus brasiliensis, des géloses trypto- caséine-soja pour Escherichia coli et des géloses de Sabouraud au dextrose pour Candida albicans. Les géloses sont incubées de 24 à 72 heures avant le comptage des colonies présentes. [0188] Samples and counts of the microorganisms are carried out at 30 minutes, 24 hours and 48 hours for each microorganism. The inoculated samples are taken, serially diluted in diluent (casein peptone 1 g/L, sodium chloride 8.5 g/L, pH 7) and deposited respectively on potato and dextrose agars for Aspergillus brasiliensis, tryptocasein-soya agars for Escherichia coli and Sabouraud dextrose agars for Candida albicans. The agars are incubated for 24 to 72 hours before counting the colonies present.
[0189]Les mesures de populations de microorganismes réalisées à chaque temps de prélèvement sont exprimées en ufc/mL. La limite de détection du test de 100 ufc/mL. [0189] The measurements of populations of microorganisms carried out at each sampling time are expressed in cfu/mL. The detection limit of the test is 100 cfu/mL.
[0190] Les résultats des tests menés sont présentés dans le tableau 7 pour Escherichia Coli, dans le tableau 8 pour Candida Albicans, dans le tableau 9 pour Aspergillus Brasiliensis, dans le tableau 10 pour Staphylococcus Aureus, et dans le tableau 11 pour Pseudomonas Aeruginosa. The results of the tests carried out are presented in Table 7 for Escherichia Coli, in Table 8 for Candida Albicans, in Table 9 for Aspergillus Brasiliensis, in Table 10 for Staphylococcus Aureus, and in Table 11 for Pseudomonas Aeruginosa. .
[Tableau 7] : E.Coli [Table 7]: E.Coli
[0191][Tableau 8] : C.AIbicans [0191][Table 8]: C.AIbicans
[0192] [Tableau 9] : A.Brasiliensis [0192] [Table 9]: A. Brasiliensis
[0193] [Tableau 10] : S. Aureus [0193] [Table 10]: S. Aureus
[0194] [Tableau 11 ] : P. Aeruginosa [0194] [Table 11 ]: P. aeruginosa
[0195]Tous ces résu tats montrent que les compositions 40 et 43 ont des propriétés antibactériennes et antifongiques en conditions de culture in-vitro sur milieu de type gélose, car elles permettent de stabiliser microbiologiquement des milieux de cultures inoculés avec les bactéries et les champignons de référence sur des durées allant jusqu’à 48 heures. [0195] All these results show that compositions 40 and 43 have antibacterial and antifungal properties under in vitro culture conditions on agar-type medium, because they make it possible to microbiologically stabilize culture media inoculated with bacteria and fungi. reference for periods of up to 48 hours.
[0196] Avantageusement toujours, les compositions antimicrobiennes gardent leurs propriétés antifongiques et antibactériennes une fois intégrées dans des compositions cosmétiques. [0196] Still advantageously, the antimicrobial compositions retain their antifungal and antibacterial properties once incorporated into cosmetic compositions.
[0197] Exemple 4 : activation de conservateurs à pH 6 dans une émulsion huile-dans- eau Example 4: activation of preservatives at pH 6 in an oil-in-water emulsion
[0198] Dans cet exemple, on démontre la capacité de la composition 43 préparée à l’exemple 3, à activer, l’activité bactéricide et fongicide de conservateurs à pH 6 dans une émulsion huile-dans-eau. Les conservateurs sont le phenoxyéthanol, l’alcool benzylique, le benzoate de sodium, et le sorbate de potassium. Ils sont listés sur l’annexe 5 du règlement n°1223/2009. In this example, the ability of composition 43 prepared in Example 3 to activate the bactericidal and fungicidal activity of preservatives at pH 6 in an oil-in-water emulsion is demonstrated. The preservatives are phenoxyethanol, benzyl alcohol, sodium benzoate, and potassium sorbate. They are listed in appendix 5 of regulation no. 1223/2009.
[0199] Le produit cosmétique utilisé pour cette démonstration est une crème de type émulsion huile-dans-eau, dite « crème coton ». Des crèmes sont préparées selon la composition du tableau 12, en ajoutant les quantités suffisantes, notées « Qs », de composition 43 et de conservateur selon les valeurs du tableau 10. On réalise des tests d’efficacité de la protection antimicrobienne sur chaque crème du tableau 13 pour les cinq microorganismes de la norme ISO 11930 :2019 Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Candida Albicans, Aspergillus Brasiliensis. The cosmetic product used for this demonstration is a cream of the oil-in-water emulsion type, called “cotton cream”. Creams are prepared according to the composition of table 12, by adding sufficient quantities, denoted "Qs", of composition 43 and preservative according to the values of table 10. antimicrobial protection efficacy tests on each cream in table 13 for the five microorganisms of the ISO 11930:2019 standard Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Candida Albicans, Aspergillus Brasiliensis.
[0200] [Tableau 12] [0200] [Table 12]
[0201] Pour préparer la crème du tableau 9, on mélange à part tous les ingrédients de la phase A et on chauffe à 75°C. En maintenant à 75°C, on ajoute la phase B dans la phase A sous agitation douce (500-750 rpm ; hélice marine), et on attend que le mélange soit homogène. Puis on ajoute la phase A+B dans la phase C sous agitation émulsifiante (3000 rpm ; défloculeuse) pendant 10 minutes, en maintenant à 75°C. On laisse refroidir à 45°C, et on ajoute la phase D sous agitation moyenne (1500 rpm ; hélice marine). On refroidit à 25°C sous agitation douce (500-750 rpm ; hélice marine), puis on ajuste enfin le pH à 6 avec la phase E. To prepare the cream of Table 9, all the ingredients of phase A are mixed separately and heated to 75°C. While maintaining at 75° C., phase B is added to phase A with gentle stirring (500-750 rpm; marine propeller), and the mixture is waited for to be homogeneous. Then phase A+B is added to phase C with emulsifying stirring (3000 rpm; deflocculating) for 10 minutes, maintaining at 75°C. The mixture is allowed to cool to 45° C., and phase D is added with moderate stirring (1500 rpm; marine propeller). The mixture is cooled to 25° C. with gentle stirring (500-750 rpm; marine propeller), then the pH is finally adjusted to 6 with phase E.
[0202] [Tableau 13] [0202] [Table 13]
[0203] Chaque test d’efficacité de protection antimicrobienne est conduit selon les directives de la norme ISO 11930 :2019. Les résultats sont fournis dans les tableaux 14 à 19. Ils sont exprimés en réduction logarithmique de nombres d’unités formant colonies par mL. Une valeur positive correspond à une diminution du nombre d’unités formant colonies. Une valeur négative correspond à une augmentation du nombre d’unité formant colonies. [0203] Each antimicrobial protection efficacy test is conducted according to the guidelines of the ISO 11930:2019 standard. The results are provided in Tables 14 to 19. They are expressed as the logarithmic reduction in the number of colony forming units per mL. A positive value corresponds to a decrease in the number of colony forming units. A negative value corresponds to an increase in the number of colony forming units.
[0204] [Tableau 14] [0204] [Table 14]
[0205] La mesure de protection antimicrobienne de la crème 1 , qui est une crème sans aucun conservateur et sans activateur de conservateur, montre que la crème 1 n’est pas protégée contre Pseudomonas Aeruginosa, Escherichia Coli, et Candida Albicans, mais est protégée contre Staphylococcus Aureus et Aspergillus Brasiliensis (on parle d’autoprotection) au-delà de 14 jours. Cette mesure constitue notre témoin négatif. [0205] The antimicrobial protection measure of cream 1, which is a cream without any preservative and without preservative activator, shows that cream 1 is not protected against Pseudomonas Aeruginosa, Escherichia Coli, and Candida Albicans, but is protected against Staphylococcus Aureus and Aspergillus Brasiliensis (we speak of self-protection) beyond 14 days. This measurement is our negative control.
[0206] La mesure de la protection antimicrobienne de la crème 2, qui contient 1 % en poids de conservateur Microcare® PM4 de Thor, est protégée contre tous les cinq micro-organismes. Cette mesure constitue notre témoin positif. [0206] The antimicrobial protection measure of Cream 2, which contains 1% by weight of Thor's Microcare® PM4 preservative, is protected against all five microorganisms. This measurement is our positive control.
[0207] [Tableau 15] [0207] [Table 15]
[0208] Les mesures de protection antimicrobienne des crèmes 3 et 4, qui contiennent respectivement 1 % et 1 ,5% de composition 43, et aucun conservateur, montrent qu’aucune de ces crèmes n’est protégée contre Pseudomonas Aeruginosa et Candida Albicans. L’autoprotection contre Staphylococcus Aureus et Aspergillus Brasiliensis est maintenue. Concernant Escherichia Coli, une protection est observée à partir de 28 jours. La composition 43 ne permet pas de protéger la crème contre le développement microbien. Il est toutefois notable que la composition 43 ne dégrade pas l’autoprotection de la crème contre Staphylococcus Aureus et Aspergillus Brasiliensis. [0208] The antimicrobial protection measures of creams 3 and 4, which contain 1% and 1.5% of composition 43 respectively, and no preservative, show that none of these creams is protected against Pseudomonas Aeruginosa and Candida Albicans. Self-protection against Staphylococcus Aureus and Aspergillus Brasiliensis is maintained. Concerning Escherichia Coli, protection is observed from 28 days. Composition 43 does not make it possible to protect the cream against microbial development. It is however notable that composition 43 does not degrade the self-protection of the cream against Staphylococcus Aureus and Aspergillus Brasiliensis.
[0209] [Tableau 16] [0209] [Table 16]
[0210] Concernant la crème 5, la protection microbienne conférée par 0,4 % en poids de phénoxyéthanol permet de protéger la crème mais insuffisamment, notamment vis- à-vis de Candida albicans dont la population a pu croître en nombre et semble stabilisée, et de Aspergillus brasiliensis dont la population est peu réduite en nombre, et de manière inférieure au témoin positif. [0210] Concerning cream 5, the microbial protection conferred by 0.4% by weight of phenoxyethanol makes it possible to protect the cream but insufficiently, in particular against Candida albicans whose population has been able to increase in number and seems to have stabilized, and Aspergillus brasiliensis, the population of which is slightly reduced in number, and less than the positive control.
[0211]Concernant la crème 6, qui contient 0,4 % en poids de phénoxyéthanol et 1 % en poids de composition 43, on constate que la protection microbienne contre Pseudomonas Aeruginosa, Escherichia Coli, et Aspergillus brasiliensis est bien meilleure que celle de la crème 5, et équivalente au témoin positif. En effet, dès 7 jours, ou 14 jours pour Aspergillus Brasiliensis, de fortes réductions logarithmiques sont mesurées, et sont supérieures aux réductions mesurées sur la crème 5 d’au moins 2 log. Ces réductions se poursuivent ou se maintiennent à 14 jours et 28 jours pour Escherichia Coli et Aspergillus Brasiliensis, mais pas pour Pseudomonas Aeruginosa dont la population a pu croitre d’environ un logarithme entre 14 jours et 28 jours. L’autoprotection contre Staphylococcus aureus est maintenue. La crème 6 n’est cependant pas protégée contre Candida albicans, qui continue à s’y développer. [0211]As regards cream 6, which contains 0.4% by weight of phenoxyethanol and 1% by weight of composition 43, it is found that the microbial protection against Pseudomonas Aeruginosa, Escherichia Coli, and Aspergillus brasiliensis is much better than that of the cream 5, and equivalent to the positive control. Indeed, from 7 days, or 14 days for Aspergillus Brasiliensis, strong logarithmic reductions are measured, and are greater than the reductions measured on cream 5 by at least 2 log. These reductions continue or are maintained at 14 days and 28 days for Escherichia Coli and Aspergillus Brasiliensis, but not for Pseudomonas Aeruginosa whose population may have increased by approximately one logarithm between 14 days and 28 days. Self-protection against Staphylococcus aureus is maintained. However, Cream 6 is not protected against Candida albicans, which continues to grow there.
[0212] Avantageusement, la composition 43 permet donc d’activer le pouvoir conservateur du phénoxyéthanol vis-à-vis de Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis et Staphylococcus aureus. [0212] Advantageously, composition 43 therefore makes it possible to activate the preservative power of phenoxyethanol against Pseudomonas Aeruginosa, Escherichia Coli, Aspergillus brasiliensis and Staphylococcus aureus.
[0213] [Tableau 17] [0213] [Table 17]
[0214] Concernant la crème 7, la protection microbienne conférée par 0,4 % en poids d’alcool benzylique ne permet pas protéger la crème. Notamment, l’alcool benzylique dégrade fortement (de plus de 2 log à 14 jours) l’autoprotection de la crème coton contre Staphylococcus aureus. [0214] Concerning cream 7, the microbial protection conferred by 0.4% by weight of benzyl alcohol does not make it possible to protect the cream. In particular, benzyl alcohol strongly degrades (by more than 2 log at 14 days) the self-protection of cotton cream against Staphylococcus aureus.
[0215] Concernant la crème 8, qui contient 0,4 % en poids d’alcool benzylique et 1 % en poids de composition 43, on constate que la protection microbienne contre Pseudomonas Aeruginosa, Escherichia Coli, et Staphylococcus Aureus est bien meilleure que celle de la crème 7, et équivalente au témoin positif. En effet, dès 7 jours, ou 14 jours, des réductions logarithmiques significatives ou fortes sont mesurées, et sont supérieures aux réductions mesurées sur la crème 7, d’au moins 2 log pour Pseudomonas Aeruginosa et Escherichia Coli et Staphylococcus Aureus. Ces réductions se poursuivent ou se maintiennent à 14 jours et à 28 jours. La crème 8 n’est cependant pas protégée contre Candida albicans, qui continue à s’y développer. Concerning cream 8, which contains 0.4% by weight of benzyl alcohol and 1% by weight of composition 43, it is found that the microbial protection against Pseudomonas Aeruginosa, Escherichia Coli, and Staphylococcus Aureus is well better than that of cream 7, and equivalent to the positive control. Indeed, from 7 days, or 14 days, significant or strong logarithmic reductions are measured, and are greater than the reductions measured on cream 7, by at least 2 log for Pseudomonas Aeruginosa and Escherichia Coli and Staphylococcus Aureus. These reductions continue or are maintained at 14 days and 28 days. However, Cream 8 is not protected against Candida albicans, which continues to grow there.
[0216] Avantageusement, la composition 43 permet donc d’activer le pouvoir conservateur de l’alcool benzylique vis-à-vis de Pseudomonas Aeruginosa, Escherichia Coli, et Staphylococcus Aureus. Advantageously, composition 43 therefore makes it possible to activate the preservative power of benzyl alcohol against Pseudomonas Aeruginosa, Escherichia Coli, and Staphylococcus Aureus.
[0217] [Tableau 18] [0217] [Table 18]
[0218] Concernant la crème 9, la protection microbienne conférée par 0,4 % en poids de benzoate de sodium permet de faiblement protéger la crème, sauf contre Candida albicans. Le benzoate de sodium dégrade légèrement l’autoprotection de la crème coton contre Staphylococcus aureus. [0218] Concerning cream 9, the microbial protection conferred by 0.4% by weight of sodium benzoate provides weak protection for the cream, except against Candida albicans. Sodium benzoate slightly degrades the self-protection of cotton cream against Staphylococcus aureus.
[0219] Concernant la crème 10, qui contient 0,4 % en poids de benzoate de sodium et 1 % en poids de composition 43, on constate que la protection microbienne contre Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis et Candida albicans est bien meilleure que celle de la crème 9, et équivalente au témoin positif. En effet, dès 7 jours, ou 14 jours pour A. brasiliensis, des réductions logarithmiques significatives ou fortes sont mesurées, et sont supérieures aux réductions mesurées sur la crème 7 d’au moins 1 ou 2 log. Ces réductions se poursuivent ou se maintiennent à 14 jours et 28 jours. L’autoprotection contre Staphylococcus aureus est maintenue. Il est notable que la crème 10 présente ici une protection suffisante contre Candida albicans. [0219] Regarding cream 10, which contains 0.4% by weight of sodium benzoate and 1% by weight of composition 43, it is found that the microbial protection against Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis and Candida albicans is much better than that of cream 9, and equivalent to the positive control. Indeed, from 7 days, or 14 days for A. brasiliensis, significant or strong logarithmic reductions are measured, and are greater than the reductions measured on cream 7 by at least 1 or 2 log. These reductions continue or are maintained at 14 days and 28 days. Self-protection against Staphylococcus aureus is maintained. It is noteworthy that the cream 10 here presents sufficient protection against Candida albicans.
[0220] La composition 43 permet donc d’activer le pouvoir conservateur du benzoate de sodium vis-à-vis de Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis, et Candida albicans. La combinaison de 1 % (en poids) de la composition 43 et de 0,4% (en poids) du benzoate de sodium permet de stabiliser la crème selon le critère B de la norme ISO 11930 :2019. [0220]Composition 43 therefore makes it possible to activate the preservative power of sodium benzoate against Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Aspergillus brasiliensis, and Candida albicans. The combination of 1% (by weight) of composition 43 and 0.4% (by weight) of the sodium benzoate makes it possible to stabilize the cream according to criterion B of standard ISO 11930:2019.
[0221] [Tableau 19] [0221] [Table 19]
[0222] Concernant la crème 11 , la protection microbienne conférée par 0,4 % en poids de sorbate de potassium permet de protéger la crème de manière équivalente au témoin positif, sauf contre Pseudomonas aeruginosa (dès 7 jours), Escherichia Coli (à 7 jours) et Candida Albicans (à 28 jours). [0222] Concerning the cream 11 , the microbial protection conferred by 0.4% by weight of potassium sorbate makes it possible to protect the cream in an equivalent manner to the positive control, except against Pseudomonas aeruginosa (from 7 days), Escherichia Coli (at 7 days) and Candida Albicans (at 28 days).
[0223] Concernant la crème 12, qui contient 0,4 % en poids de sorbate de potassium et 1 % en poids de composition 43, on constate que la protection microbienne contre Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Candida Albicans et Aspergillus brasiliensis est bien meilleure que celle de la crème 11 , et même meilleure que celle de la crème 2 témoin positif (contenant 1 % de Microcare® PM4). En effet, dès 7 jours, ou 14 jours pour Aspergillus Brasiliensis, de fortes réductions logarithmiques sont mesurées, et sont supérieures aux réductions mesurées sur la crème 11 d’au moins 2 log. Ces réductions se maintiennent ou se poursuivent à 14 jours et 28 jours. [0224]Avantageusement, la composition 43 permet donc bien d’activer le pouvoir conservateur du sorbate de potassium vis-à-vis de Pseudomonas Aeruginosa, Escherichia Coli, Candida Albicans, Staphylococcus Aureus et Aspergillus brasiliensis. La combinaison de 1 % (en poids) de la composition 43 et de 0,4% (en poids) du sorbate de potassium permet de stabiliser la crème selon le critère A de la norme ISO 11930 :2019. [0223] Regarding cream 12, which contains 0.4% by weight of potassium sorbate and 1% by weight of composition 43, it is found that the microbial protection against Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Candida Albicans and Aspergillus brasiliensis is much better than that of cream 11 , and even better than that of positive control cream 2 (containing 1% of Microcare® PM4). Indeed, from 7 days, or 14 days for Aspergillus Brasiliensis, strong logarithmic reductions are measured, and are greater than the reductions measured on cream 11 by at least 2 log. These reductions are maintained or continue at 14 days and 28 days. [0224] Advantageously, composition 43 therefore makes it possible to activate the preservative power of potassium sorbate against Pseudomonas Aeruginosa, Escherichia Coli, Candida Albicans, Staphylococcus Aureus and Aspergillus brasiliensis. The combination of 1% (by weight) of composition 43 and 0.4% (by weight) of potassium sorbate makes it possible to stabilize the cream according to criterion A of standard ISO 11930:2019.
[0225] Exemple 5 : produits cosmétiques comprenant la composition « activateur de conservateur » et un conservateur [0225] Example 5: cosmetic products comprising the “preservative activator” composition and a preservative
[0226] Produit 1 : shampoing [0226] Product 1: shampoo
[0227] [Tableau 22] [0227] [Table 22]
[0228] Un shampoing est préparé selon la composition du tableau 22 : A shampoo is prepared according to the composition of table 22:
[0229]- On ajoute la gomme de xanthane à l’eau sous agitation moyenne jusqu’à obtenir un gel homogène, approximativement après 20 minutes d’agitation. A température de 20-22°C, on ajoute successivement les ingrédients de la phase B, sous agitation moyenne. On ajoute ensuite la phase C, toujours sous agitation douce. Puis on ajuste le pH à 4,8 avec l’acide citrique, encore sous agitation douce.- On obtient un gel fluide, transparent, et moussant. La viscosité Brookfield à 20 rpm 20°C pendant 1 minute (avec le mobile RV M04) est de 3200 mPa.s +/-500. La composition 43 est donc bien hautement compatible avec les ingrédients du shampoing. D’autres shampoings sont préparés en changeant la nature des ingrédients de la phase C selon le tableau 23. [0229]- The xanthan gum is added to the water with moderate stirring until a homogeneous gel is obtained, after approximately 20 minutes of stirring. At a temperature of 20-22° C., the ingredients of phase B are successively added, with moderate stirring. Phase C is then added, still with gentle stirring. Then the pH is adjusted to 4.8 with citric acid, again with gentle stirring. A fluid, transparent, foaming gel is obtained. The Brookfield viscosity at 20 rpm 20° C. for 1 minute (with the RV M04 spindle) is 3200 mPa.s +/-500. Composition 43 is therefore indeed highly compatible with the ingredients of the shampoo. others shampoos are prepared by changing the nature of the ingredients of phase C according to table 23.
[0230] [Tableau 23] [0230] [Table 23]
[0231]On réalise des tests d’efficacité de la protection antimicrobienne sur chaque shampoing du tableau 23 pour les cinq microorganismes de la norme ISO 11930 :2019 Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Candida Albicans, Aspergillus Brasiliensis. Les résultats sont présentés dans le tableau 24. [0231] Antimicrobial protection efficacy tests are carried out on each shampoo in table 23 for the five microorganisms of the ISO 11930:2019 standard Pseudomonas Aeruginosa, Staphylococcus Aureus, Escherichia Coli, Candida Albicans, Aspergillus Brasiliensis. The results are shown in Table 24.
[0232] [Tableau 24] [0232] [Table 24]
témoin est auto-protégée contre Staphylococcus Aureus et Escherichia Coli. Dans le shampoing 1 , le sorbate de potassium, qui est un conservateur listé, exerce un effet protecteur contre trois micro-organismes Pseudomonas Aeruginosa, Candida Albicans et Aspergillus Brasiliensis, mais fait disparaître l’autoprotection de la formule contre Escherichia Coli, la rendant non protégée contre cette dernière bactérie. Dans le shampoing 2, dans laquelle les 0,4 % de sorbate de potassium ont été substitués par 1 % de composition 43, les trois souches Pseudomonas Aeruginosa, Candida Albicans et Aspergillus Brasiliensis peuvent se développer, mais pas Escherichia Coli, dont la réduction est de 4,80 log dès sept jours. Dans cette formule de shampoing, la composition 43 permet donc d’exercer une activité antibactérienne ciblée sur la souche Escherichia Coli efficace dès sept jours et jusqu’à 28 jours. control is self-protected against Staphylococcus Aureus and Escherichia Coli. In the shampoo 1 , potassium sorbate, which is a listed preservative, exerts a protective effect against three microorganisms Pseudomonas Aeruginosa, Candida Albicans and Aspergillus Brasiliensis, but destroys the self-protection of the formula against Escherichia Coli, making it non protected against this last bacterium. In shampoo 2, in which the 0.4% potassium sorbate has been substituted by 1% of composition 43, the three strains Pseudomonas Aeruginosa, Candida Albicans and Aspergillus Brasiliensis can grow, but not Escherichia Coli, whose reduction is of 4.80 log from seven days. In this shampoo formula, composition 43 therefore makes it possible to exert an antibacterial activity targeted on the Escherichia Coli strain effective from seven days and up to 28 days.
[0234] Dans le shampoing 3, qui contient 0,4 % de sorbate de potassium et 1 % de composition 43, les effets antimicrobiens sur Pseudomonas Aeruginosa, Candida Albicans et Aspergillus Brasiliensis sont retrouvés, et aussi l’effet antibactérien sur Escherichia Coli, efficace dès 14 jours et jusque 28 jours. La composition 43 permet ainsi de protéger le shampoing contre le développement des bactéries du genre Escherichia Coli, et cela sans réduire ou perturber l’activité antimicrobienne du conservateur qu’est le sorbate de potassium mais au contraire en activant l’activité antimicrobienne du sorbate de potassium vis-à-vis de Escherichia Coli à 14 jours avec une réduction de plus de 4 logs supérieure à la réduction permise par le sorbate de potassium seul. [0234] In shampoo 3, which contains 0.4% potassium sorbate and 1% composition 43, the antimicrobial effects on Pseudomonas Aeruginosa, Candida Albicans and Aspergillus Brasiliensis are found, and also the antibacterial effect on Escherichia Coli, effective from 14 days and up to 28 days. Composition 43 thus makes it possible to protect the shampoo against the development of bacteria of the genus Escherichia Coli, and this without reducing or disturbing the antimicrobial activity of the preservative which is potassium sorbate, but on the contrary by activating the antimicrobial activity of potassium sorbate. potassium against Escherichia Coli at 14 days with a reduction of more than 4 logs greater than the reduction allowed by potassium sorbate alone.

Claims

REVENDICATIONS
1. Utilisation d’une composition liquide antimicrobienne pour activer les conservateurs de produits cosmétiques, ladite composition liquide antimicrobienne comprenant : 1. Use of an antimicrobial liquid composition for activating cosmetic product preservatives, said antimicrobial liquid composition comprising:
- Au moins une huile essentielle choisie parmi les huiles essentielles d’espèces du genre Cymbopogon, les huiles essentielles de clou de girofle, de géranium Bourbon, de laurier noble, de litsée citronnée, de mélisse, de piment, de piment couronné, d’origan, d’arbre à thé, de thym, de schénanthe ou un mélange de ces huiles; - At least one essential oil chosen from the essential oils of species of the genus Cymbopogon, the essential oils of clove, Bourbon geranium, noble laurel, lemony litsea, lemon balm, pepper, crown pepper, oregano, tea tree, thyme, lemongrass or a mixture of these oils;
- Au moins un tensioactif non-ionique choisi parmi les alkyl(poly)glycosides, les alkylglycosides, les esters d’huiles végétales, les esters gras non éthoxylés de polyols, les hétéropolymères d’alkylglycosides en C8-C10 et d’esters gras de sorbitan, ou leurs mélanges, - At least one nonionic surfactant chosen from alkyl(poly)glycosides, alkylglycosides, esters of vegetable oils, non-ethoxylated fatty esters of polyols, heteropolymers of C8-C10 alkylglycosides and fatty esters of sorbitan, or mixtures thereof,
- Au moins un acide carboxylique sous forme libre. - At least one carboxylic acid in free form.
2. Utilisation selon la revendication 1 , caractérisé en ce que les conservateurs sont choisis parmi l’acide propionique, le propionate de calcium, le formaldéhyde, le paraformaldéhyde, l’o-phenylphenol ou ses sels, le zinc pyrithione, les sulfites, bisulfites ou métabisulfites de sodium, d’ammonium, de potassium, le chlorobutanol, le méthylparaben, l’éthylparaben, le propylparaben, le butylparaben, l’acide formique et ses sels tels que le formate de sodium, l’acide benzoïque et ses sels tels que le benzoate de sodium, l’acide sorbique et ses sels , tels que le sorbate de calcium, le sorbate de sodium, le sorbate de potassium, l’acide salicylique et ses sels, l’acide déhydroacétique et ses sels tels que le déhydroacétate de sodium, l’acide undécylénique et ses sels tels que l’undécylénate de calcium, l’undécylénate de potassium, l’undécylénate de sodium, le phenoxyéthanol, le 1 ,2-Dimethylol-5,6- dimethylhydantoine, l’alcool benzylique, le chlorhexidine, le diacetate de chlorhexidine, le digluconate de chlorhexidine, le dihydrochlorure de chlorhexidine, le chlorure de behentrimonium, le chlorure de cetrimonium, le bromure de cetrimonium, le chlorure de laurtrimonium, le bromure de laurtrimonium, le chlorure de steartrimonium, le bromure de steartrimonium, l’hexamidine, le diisethionate d hexamidme, le chlorphenesin, le chlorure de benzalkonium, le bromure de benzalkonium, le saccharinate de benzalkonium,!’ éthyl lauroyl arginate. 2. Use according to claim 1, characterized in that the preservatives are chosen from propionic acid, calcium propionate, formaldehyde, paraformaldehyde, o-phenylphenol or its salts, zinc pyrithione, sulphites, bisulphites or sodium, ammonium, potassium metabisulfites, chlorobutanol, methylparaben, ethylparaben, propylparaben, butylparaben, formic acid and its salts such as sodium formate, benzoic acid and its salts such as sodium benzoate, sorbic acid and its salts, such as calcium sorbate, sodium sorbate, potassium sorbate, salicylic acid and its salts, dehydroacetic acid and its salts such as dehydroacetate sodium, undecylenic acid and its salts such as calcium undecylenate, potassium undecylenate, sodium undecylenate, phenoxyethanol, 1,2-dimethylol-5,6-dimethylhydantoin, benzyl alcohol , chlorhexidine, chlorhexidine diacetate, chlorhexidine digluconate, chlorhexidine dihydrochloride, behentrimonium chloride, cetrimonium chloride, cetrimonium bromide, laurtrimonium chloride, laurtrimonium bromide, steartrimonium chloride, steartrimonium bromide, hexamidine, diisethionate d hexamidme, chlorphenesin, benzalkonium chloride, benzalkonium bromide, benzalkonium saccharinate,!' ethyl lauroyl arginate.
3. Utilisation selon la revendication 1 ou 2, caractérisée en ce que les conservateurs sont choisis l’acide benzoique et ses sels, l’acide sorbique et ses sels, le phénoxyéthanol, l’alcool benzylique et ses sels. 3. Use according to claim 1 or 2, characterized in that the preservatives are chosen benzoic acid and its salts, sorbic acid and its salts, phenoxyethanol, benzyl alcohol and its salts.
4. Utilisation selon l’une quelconque des revendications 1 à 3, caractérisée en ce que l’huile essentielle est choisie parmi les huiles essentielles d’espèces du genre Cymbopogon, de litsée citronnée et de mélisse. 4. Use according to any one of claims 1 to 3, characterized in that the essential oil is chosen from the essential oils of species of the genus Cymbopogon, lemon beds and lemon balm.
5. Utilisation selon l’une quelconque des revendications 1 à 4, caractérisée en ce que l’huile essentielle est choisi parmi Cymbopogon flexuosus Stapf. et Cymbopogon citratus (DC.) Stapf.. 5. Use according to any one of claims 1 to 4, characterized in that the essential oil is chosen from Cymbopogon flexuosus Stapf. and Cymbopogon citratus (DC.) Stapf..
6. Utilisation selon l’une quelconque des revendications 1 à 4, caractérisée en ce que le tensioactif non-ionique est choisi parmi les alkyl(poly)glucosides. 6. Use according to any one of claims 1 to 4, characterized in that the nonionic surfactant is chosen from alkyl (poly) glucosides.
7. Utilisation selon l’une quelconque des revendications 1 à 6, caractérisée en ce que le tensioactif non-ionique est choisi parmi les décylglucosides, les dodécylglucosides, les hetpoglucosides, les caprylyl glucosides, les capryl glucosides et les caprylyl/capryl glucosides. 7. Use according to any one of claims 1 to 6, characterized in that the nonionic surfactant is chosen from decylglucosides, dodecylglucosides, hetpoglucosides, caprylyl glucosides, capryl glucosides and caprylyl/capryl glucosides.
8. Utilisation selon l’une quelconque des revendications 1 à 7, caractérisée en ce que le rapport de la masse sèche totale de tensioactifs non ioniques sur la masse sèche totale d’huiles essentielles est supérieur ou égal à 2. 8. Use according to any one of claims 1 to 7, characterized in that the ratio of the total dry mass of nonionic surfactants to the total dry mass of essential oils is greater than or equal to 2.
9. Utilisation selon l’une quelconque des revendications 1 à 8, caractérisée en ce l’acide carboxylique sous forme libre est choisi parmi l’acide gluconique, l’acide glucuronique, l’acide maltobionique, l’acide succinique, l’acide glucarique, et l’acide glutarique. 9. Use according to any one of claims 1 to 8, characterized in that the carboxylic acid in free form is chosen from gluconic acid, glucuronic acid, maltobionic acid, succinic acid, acid glucaric, and glutaric acid.
10. Utilisation selon l’une quelconque des revendications 1 à 9, caractérisée en ce l’acide carboxylique sous forme libre est l’acide gluconique. 10. Use according to any one of claims 1 to 9, characterized in that the carboxylic acid in free form is gluconic acid.
11 . Utilisation selon l’une quelconque des revendications 1 à 10, caractérisée en ce que la composition antimicrobienne comprend en outre au moins un sel d’acide carboxylique choisi parmi les sels de sodium, de magnésium, de zinc, de calcium, de potassium, de fer, de lithium. 11 . Use according to any one of Claims 1 to 10, characterized in that the antimicrobial composition additionally comprises at least one carboxylic acid salt chosen from the salts of sodium, magnesium, zinc, calcium, potassium, iron, lithium.
12. Utilisation selon l’une quelconque des revendications 1 a 11 , caractérisée en ce que le sel d’acide carboxylique est le gluconate de sodium. 12. Use according to any one of claims 1 to 11, characterized in that the carboxylic acid salt is sodium gluconate.
13. Composition liquide antimicrobienne comprenant : 13. Antimicrobial liquid composition comprising:
- de l’huile essentielle d’une des espèces du genre Cymbopogon, - essential oil of one of the species of the genus Cymbopogon,
- du caprylyl/capryl glucoside, - caprylyl/capryl glucoside,
- de l’acide gluconique, - gluconic acid,
- du gluconate de sodium, - sodium gluconate,
- de l’eau. - some water.
14. Composition selon la revendication 13, caractérisée en ce que : 14. Composition according to claim 13, characterized in that:
- l’huile essentielle d’une des espèces du genre Cymbopogon est présente à un pourcentage massique allant de 0,1% à 10% en poids sec, - the essential oil of one of the species of the Cymbopogon genus is present at a mass percentage ranging from 0.1% to 10% by dry weight,
- le caprylyl/capryl glucoside est présent à un pourcentage massique allant de 1 % à 40% en poids sec, - the caprylyl/capryl glucoside is present at a mass percentage ranging from 1% to 40% by dry weight,
- l’acide gluconique libre est présent à un pourcentage massique allant de 10% à 70% en poids sec, - free gluconic acid is present at a mass percentage ranging from 10% to 70% by dry weight,
- le gluconate de sodium est présent à un pourcentage massique allant de 1 % à 50% en poids sec, - the sodium gluconate is present at a mass percentage ranging from 1% to 50% by dry weight,
- l’eau présente à un pourcentage massique allant de 20% à 75% en poids, les pourcentages massiques étant exprimés par rapport au poids total de la composition liquide antimicrobienne. - the water present at a mass percentage ranging from 20% to 75% by weight, the mass percentages being expressed relative to the total weight of the antimicrobial liquid composition.
15. Produit cosmétique caractérisé en ce qu’il comprend : 15. Cosmetic product characterized in that it comprises:
- -jusqu’à 2,5 % en poids brut, d’au moins un conservateur, choisi parmi l’acide benzoique et ses sels, l’acide sorbique et ses sels, le phénoxyéthanol, l’alcool benzylique et ses sels , - -up to 2.5% by gross weight, of at least one preservative, chosen from benzoic acid and its salts, sorbic acid and its salts, phenoxyethanol, benzyl alcohol and its salts,
- et au moins 1 % en poids brut d’une composition liquide antimicrobienne selon les revendications 13 ou 14, par rapport au poids total du produit cosmétique. - and at least 1% by gross weight of a liquid antimicrobial composition according to claims 13 or 14, relative to the total weight of the cosmetic product.
16. Produit cosmétique selon la revendication 15, caractérisé en ce qu’il est sous forme d’une émulsion huile-dans-eau, ou d’une émulsion eau-dans-huile, ou d’une suspension aqueuse, ou d’une mousse aqueuse, ou d’une solution aqueuse vraie, ou d’une solution micellaire, ou d’une solution hydroalcoolique, ou d’une pâte, ou d’un gel, ou d’une poudre, ou d’un comprimé, ou d’une lingette. 16. Cosmetic product according to claim 15, characterized in that it is in the form of an oil-in-water emulsion, or of a water-in-oil emulsion, or of an aqueous suspension, or of a aqueous foam, or a true aqueous solution, or a micellar solution, or a hydroalcoholic solution, or a paste, or a gel, or a powder, or a tablet, or of a wipe.
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US5403587A (en) 1993-04-22 1995-04-04 Eastman Kodak Company Disinfectant and sanitizing compositions based on essential oils
US6346281B1 (en) 2000-05-05 2002-02-12 Scentsible Life Products, A Division Of Laid Back Designs Ltd. Antimicrobial composition formulated with essential oils
US20080253976A1 (en) 2007-04-16 2008-10-16 Douglas Craig Scott Personal Care Compositions Comprising An Antimicrobial Blend of Essential Oils or Constituents Thereof
US20100114146A1 (en) 2008-10-30 2010-05-06 Albrecht Thomas E Methods and devices for predicting intra-gastric satiety and satiation creation device system performance
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