FR2945936A1 - Preparing aqueous emulsion of oily active substance, useful for e.g. cosmetic and food use, comprises mixing hydrophilic component (water and saponin emulsifier), mixing lipophilic components (substance and stabilizer) and homogenizing - Google Patents

Preparing aqueous emulsion of oily active substance, useful for e.g. cosmetic and food use, comprises mixing hydrophilic component (water and saponin emulsifier), mixing lipophilic components (substance and stabilizer) and homogenizing Download PDF

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FR2945936A1
FR2945936A1 FR0902520A FR0902520A FR2945936A1 FR 2945936 A1 FR2945936 A1 FR 2945936A1 FR 0902520 A FR0902520 A FR 0902520A FR 0902520 A FR0902520 A FR 0902520A FR 2945936 A1 FR2945936 A1 FR 2945936A1
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stabilizer
emulsion
active substance
emulsifier
aqueous emulsion
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Jean Claude Epiphani
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    • 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
    • A61K8/068—Microemulsions
    • 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
    • A61K8/31—Hydrocarbons
    • 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
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/06—Ointments; Bases therefor; Other semi-solid forms, e.g. creams, sticks, gels
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K9/00—Medicinal preparations characterised by special physical form
    • A61K9/10—Dispersions; Emulsions
    • A61K9/107—Emulsions ; Emulsion preconcentrates; Micelles
    • A—HUMAN NECESSITIES
    • A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
    • A61Q19/00—Preparations for care of the skin
    • 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
    • A61K2800/20—Chemical, physico-chemical or functional or structural properties of the composition as a whole
    • A61K2800/30—Characterized by the absence of a particular group of ingredients
    • A61K2800/33—Free of surfactant

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  • Health & Medical Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Animal Behavior & Ethology (AREA)
  • General Health & Medical Sciences (AREA)
  • Public Health (AREA)
  • Veterinary Medicine (AREA)
  • Epidemiology (AREA)
  • Chemical & Material Sciences (AREA)
  • Birds (AREA)
  • Dispersion Chemistry (AREA)
  • Pharmacology & Pharmacy (AREA)
  • Medicinal Chemistry (AREA)
  • Oil, Petroleum & Natural Gas (AREA)
  • Dermatology (AREA)
  • Colloid Chemistry (AREA)
  • Medicinal Preparation (AREA)

Abstract

Preparation of an aqueous emulsion of an oily active substance comprises: mixing hydrophilic components comprising water, and a saponin emulsifier; mixing lipophilic components comprising the oily active substance and stabilizer; and homogenizing the two mixtures by mechanical action, where the stabilizer is a noncyclic liquid hydrocarbon, with an average molecular mass of greater than 150 g. Independent claims are included for: (1) the aqueous emulsion obtained by the process; (2) a gel comprising the emulsion and a thickener; and (3) a cream containing the emulsion and the thickener.

Description

. Champ de l'invention . Field of the invention

La présente invention est relative à des émulsions aqueuses de substances actives huileuses destinées aux industries cosmétiques, alimentaires et pharmaceutiques. The present invention relates to aqueous emulsions of oily active substances for the cosmetic, food and pharmaceutical industries.

2. Etat actuel de la technique 2. Current state of the art

Dans les domaines des industries cosmétiques, alimentaires et pharmaceutiques, de nombreuses substances actives sont de type huileux, c'est à dire lipophiles ou hydrophobes : huiles végétales, huiles essentielles, concentrés de parfums, actifs huileux divers de type cosmétique, alimentaire ou pharmaceutique. II est très intéressant de réaliser des émulsions aqueuses de ces substances actives de type huileux, pour une raison essentielle : l'eau est le vecteur le mieux adapté pour le corps humain, que ce soit pour un usage externe (parfums et applications cosmétiques) ou pour un usage interne (applications alimentaires ou pharmaceutiques). In the fields of the cosmetic, food and pharmaceutical industries, many active substances are oily, that is to say lipophilic or hydrophobic: vegetable oils, essential oils, perfume concentrates, various oily active cosmetics, food or pharmaceutical. It is very interesting to make aqueous emulsions of these active substances of oily type, for an essential reason: water is the vector best suited for the human body, whether for external use (perfumes and cosmetic applications) or for internal use (food or pharmaceutical applications).

On sait depuis longtemps réaliser des émulsions huile dans eau (H / E) à l'aide d'émulsionnants chimiques divers, mais ces émulsionnants présentent des inconvénients notoires : - ils sont généralement mal supportés par le corps humain, - ils doivent être utilisés avec une concentration importante par rapport aux substances actives. It has long been known to produce oil-in-water (O / W) emulsions using various chemical emulsifiers, but these emulsifiers have notable drawbacks: they are generally poorly supported by the human body, they must be used with a significant concentration compared to the active substances.

La technologie des cyclodextrines est une autre voie possible, mais elle présente aussi plusieurs contraintes qui limitent fortement son utilisation. Cyclodextrin technology is another possible route, but it also has several constraints that severely limit its use.

On a enfin envisagé l'utilisation des saponosides, qui sont des émulsionnants végétaux appartenant à la famille des glucides (hétérosides). Une première catégorie d'applications utilise des substances auxiliaires (hydrates de carbone, éthanol,...) en quantités importantes qui dénaturent l'émulsion finale. Finally, we have considered the use of saponosides, which are plant emulsifiers belonging to the carbohydrate (heteroside) family. A first category of applications uses auxiliary substances (carbohydrates, ethanol, ...) in large quantities which denature the final emulsion.

Une deuxième catégorie d'applications n'utilise pas de substances auxiliaires mais présente en pratique l'inconvénient de fournir des émulsions instables. A second category of applications does not use auxiliary substances but in practice has the disadvantage of providing unstable emulsions.

Au total, en raison de ces limitations, les industries cosmétiques, alimentaires et pharmaceutiques fabriquent peu d'émulsions aqueuses d'actifs huileux en dépit de leur intérêt évident. All in all, because of these limitations, the cosmetic, food and pharmaceutical industries produce few aqueous emulsions of oily actives despite their obvious interest.

3. Description de l'invention Rappelons tout d'abord qu'une émulsion aqueuse est constituée majoritairement d'eau dans laquelle sont dispersées des gouttelettes d'un liquide non miscible à l'eau, les dites gouttelettes étant entourées de molécules d'une substance appelée émulsionnant . 1 La finesse de l'émulsion est caractérisée par le diamètre des gouttelettes qui est habituellement de l'ordre de grandeur du micromètre (10-6 mètre). 3. DESCRIPTION OF THE INVENTION Let us first recall that an aqueous emulsion consists mainly of water in which are dispersed droplets of a water immiscible liquid, said droplets being surrounded by molecules of a substance called emulsifier. 1 The fineness of the emulsion is characterized by the diameter of the droplets which is usually of the order of magnitude of the micrometer (10-6 meters).

Après plusieurs années de recherches et d'essais, il a été mis au point par le demandeur un procédé permettant de réaliser des émulsions aqueuses très fluides de substances actives huileuses, dans les domaines des industries cosmétiques, alimentaires et pharmaceutiques, le dit procédé éliminant les inconvénients des techniques en vigueur jusqu'à maintenant. After several years of research and testing, the applicant has developed a method for producing very fluid aqueous emulsions of oily active substances in the fields of the cosmetic, food and pharmaceutical industries, the process eliminating the disadvantages of the techniques in force until now.

Ainsi l'invention concerne un procédé de fabrication d'une émulsion aqueuse d'une substance active huileuse pour application cosmétique, alimentaire ou pharmaceutique, comprenant les étapes suivantes : - mélange de composants hydrophiles, comprenant de l'eau, un saponoside émulsionnant, - mélange de composants lipophiles, comprenant la substance active huileuse, un stabilisateur, - homogénéisation des deux mélanges par action mécanique, le stabilisateur étant un liquide hydro-carboné non cyclique, d'une masse molaire moyenne supérieure à environ 150 grammes. Thus, the invention relates to a process for producing an aqueous emulsion of an oily active substance for cosmetic, food or pharmaceutical application, comprising the following steps: a mixture of hydrophilic components, comprising water, an emulsifying saponoside, mixture of lipophilic components, comprising the oily active substance, a stabilizer, homogenization of the two mixtures by mechanical action, the stabilizer being a noncyclic hydrocarbon liquid with an average molar mass of greater than about 150 grams.

L'action mécanique d'homogénéisation doit être adaptée à la finesse requise pour l'émulsion. The mechanical homogenization action must be adapted to the fineness required for the emulsion.

Par stabilisateur, il faut entendre une substance auxiliaire qui supprime 25 l'instabilité de l'émulsion et qui ne dénature pas l'émulsion fabriquée sur le plan organoleptique. By stabilizer is meant an auxiliary substance which suppresses the instability of the emulsion and does not denature the organoleptically produced emulsion.

En l'espèce, le stabilisateur est évidemment compatible avec l'application envisagée (cosmétique, alimentaire ou pharmaceutique), c'est à dire en 30 particulier non irritant et non toxique. In this case, the stabilizer is obviously compatible with the intended application (cosmetic, food or pharmaceutical), that is to say in particular non-irritating and non-toxic.

De préférence, le stabilisateur comprend une proportion d'atomes d'oxygène inférieure à 2 atomes d'oxygène pour 10 atomes de carbone. Un exemple typique de stabilisateur est la paraffine liquide. Mais tout liquide 35 répondant à la définition ci-dessus peut être utilisé. Preferably, the stabilizer comprises a proportion of oxygen atoms of less than 2 oxygen atoms per 10 carbon atoms. A typical example of a stabilizer is liquid paraffin. But any liquid as defined above can be used.

Avantageusement, on ajoute au mélange de composants hydrophiles au moins un additif hydrophile, et au mélange de composants lipophiles, au moins un additif lipophile. 40 On entend par additifs , des substances annexes telles que des conservateurs, des anti-oxydants, des séquestrants assurant la conservation de la substance active. Advantageously, at least one hydrophilic additive is added to the mixture of hydrophilic components, and at least one lipophilic additive to the mixture of lipophilic components. Additives are adjunctive substances such as preservatives, antioxidants, sequestering agents for the preservation of the active substance.

45 En lieu et place des additifis, on peut utiliser tout autre moyen de conservation, comme par exemple une étape de stérilisation de l'ensemble de l'émulsion homogénéisée. In place of the additives, any other means of preservation may be used, such as, for example, a step of sterilizing the whole of the homogenized emulsion.

Le procédé de l'invention permet de réaliser des émulsions aqueuses très fluides comprenant plus de 40 % de substances huileuses avec moins de 2% d'émulsionnant, ce qui est irréalisable avec tout autre procédé. The process of the invention makes it possible to produce very fluid aqueous emulsions comprising more than 40% of oily substances with less than 2% of emulsifier, which is unfeasible with any other method.

Les émulsions obtenues sont toujours laiteuses. The emulsions obtained are always milky.

Les saponosides, d'origine végétale, synthétique ou semi-synthétique, ont été retenus comme émulsionnants car, dans les conditions où ils sont utilisés dans les émulsions fabriquées selon l'invention, ils présentent les avantages suivants par rapport aux émulsionnants chimiques : - ils sont parfaitement adaptés au corps humain, tant en usage externe (ils sont utilisés depuis longtemps dans des shampooings par exemple), qu'en usage interne ; - ils possèdent un fort pouvoir émulsionnant et peuvent être utilisés avec une faible concentration par rapport aux substances actives. The saponosides, of plant origin, synthetic or semi-synthetic, have been retained as emulsifiers because, under the conditions in which they are used in the emulsions manufactured according to the invention, they have the following advantages over chemical emulsifiers: are perfectly adapted to the human body, both in external use (they have been used for a long time in shampoos for example), and in internal use; they possess a high emulsifying power and can be used with a low concentration relative to the active substances.

Les saponosides d'origine végétale sont des glucides dotés de propriétés émulsionnantes, que l'on extrait de végétaux spécifiques comme la saponaire ou le savon indien. Saponosides of plant origin are carbohydrates with emulsifying properties, which are extracted from specific plants such as soapwort or Indian soap.

Il faut rappeler que les glucides sont des molécules composées d'atomes de carbone, d'hydrogène et d'oxygène, avec une proportion atomes de carbone / atomes d'oxygène comprise entre 1 et 2 environ, avec de nombreux groupes O û H. En phytochimie, les saponosides sont classés parmi les hétérosides. It should be remembered that carbohydrates are molecules composed of carbon atoms, hydrogen and oxygen, with a proportion carbon atoms / oxygen atoms of between 1 and 2 approximately, with many groups O - H. In phytochemistry, saponosides are classified as glycosides.

Ce sont des molécules complexes, de masse molaire élevée, comme C104H168O55, de masse molaire M = 2.296 g. Comme tous les émulsionnants, naturels ou synthétiques, les saponosides comprennent une extrémité hydrophile et une extrémité lipophile. Dans l'émulsion finale, la surface extérieure de chaque gouttelette de phase huileuse est tapissée de molécules de saponosides, en couche monomoléculaire, avec les extrémités hydrophiles dans l'eau et les extrémités lipophiles dans la gouttelette de phase huileuse. They are complex molecules of high molar mass, such as C104H168O55, with a molar mass M = 2.296 g. Like all natural or synthetic emulsifiers, the saponosides comprise a hydrophilic end and a lipophilic end. In the final emulsion, the outer surface of each oily phase droplet is lined with saponoside molecules, in a monomolecular layer, with the hydrophilic ends in the water and the lipophilic ends in the oily phase droplet.

Les concentrations optimales en émulsionnant et en stabilisateur doivent être déterminées par des essais préalables, vu la diversité des substances actives huileuses à émulsionner et la variété des concentrations requises. The optimum concentrations of emulsifier and stabilizer should be determined by prior testing, given the variety of oily active substances to be emulsified and the variety of concentrations required.

Dans certaines applications, il est possible ou souhaitable d'utiliser en sus des saponosides au moins un co-émulsionnant d'origine naturelle ou synthétique. In some applications, it is possible or desirable to use in addition to saponosides at least one co-emulsifier of natural or synthetic origin.

Il faut noter enfin que les émulsions de l'invention, très fluides, peuvent servir de base pour la réalisation de gels ou crèmes par addition d'épaississant(s) adaptés à l'application. 4. Exemple de fabrication d'une émulsion selon le procédé de l'invention Finally, it should be noted that the emulsions of the invention, very fluid, can be used as a basis for the production of gels or creams by adding thickeners (s) suitable for application. 4. Example of manufacture of an emulsion according to the process of the invention

Il s'agit de réaliser une émulsion aqueuse de parfum à 10 %. Les composants de l'émulsion, et leurs % masse, sont les suivants. 2945936 4 Composants hydrophiles 84,25 % - Eau déminéralisée ( phase continue) : - Saponosides purs ( émulsionnant) : 0,46 % - Benzoate de sodium ( conservateur) : 0,03 % - EDTA tétrasodique ( séquestrant) : 0,05 % Composants lipophiles 10,00 % - Concentré de parfum ( phase dispersée) : - Paraffine liquide ( stabilisateur) : 4,56 0/0 - Phenonip XB ( conservateur) : 0,60 % - BHT ( anti-oxydant) : 0,05 0/0 Total : 100,00 % 15 On mélange séparément les composants hydrophiles et les composants lipophiles pour obtenir des solutions homogènes. This is to achieve a 10% aqueous perfume emulsion. The components of the emulsion, and their% mass, are as follows. 2945936 4 Hydrophilic components 84.25% - Demineralized water (continuous phase): - Pure saponosides (emulsifier): 0.46% - Sodium benzoate (preservative): 0.03% - Tetrasodium tetra (sequestering): 0.05% Lipophilic components 10.00% - Perfume concentrate (dispersed phase): - Liquid paraffin (stabilizer): 4.56% - Phenonip XB (preservative): 0.60% - BHT (antioxidant): 0.05 0/0 Total: 100.00% The hydrophilic components and the lipophilic components are mixed separately to obtain homogeneous solutions.

On effectue l'homogénéisation des deux solutions de l'ensemble avec un mélangeur de la marque protégée Ultra-Turrax, à turbine rotor-stator, pendant 20 10 minutes à 17.500 tours / minute. The two solutions of the assembly were homogenized with a mixer of the protected trademark Ultra-Turrax, rotor-stator turbine, for 10 minutes at 17,500 revolutions / minute.

On obtient une émulsion laiteuse homogène très fluide. 25 30 35 40 5 10 45 A homogeneous milky, very fluid emulsion is obtained. 25 30 35 40 5 10 45

Claims (8)

Revendications1. Procédé de fabrication d'une émulsion aqueuse d'une substance active huileuse pour application cosmétique, alimentaire ou pharmaceutique, comprenant les étapes suivantes : - mélange de composants hydrophiles, comprenant de l'eau, un saponoside émulsionnant, - mélange de composants lipophiles, comprenant la substance active huileuse, un stabilisateur, - homogénéisation des deux mélanges par action mécanique, le stabilisateur étant un liquide hydrocarboné non cyclique, d'une masse molaire moyenne supérieure à environ 150 grammes. Revendications1. A process for the manufacture of an aqueous emulsion of an oily active substance for cosmetic, food or pharmaceutical application, comprising the following steps: a mixture of hydrophilic components, comprising water, an emulsifying saponoside, a mixture of lipophilic components, comprising: the oily active substance, a stabilizer, - homogenization of the two mixtures by mechanical action, the stabilizer being a noncyclic hydrocarbon liquid having an average molar mass of greater than about 150 grams. 2. Procédé selon la revendication 1, dans lequel on ajoute au mélange de composants hydrophiles au moins un additif hydrophile, et au mélange de composants lipophiles, au moins un additif lipophile. 2. Method according to claim 1, wherein is added to the mixture of hydrophilic components at least one hydrophilic additive, and the mixture of lipophilic components, at least one lipophilic additive. 3. Procédé selon la revendication 1, dans lequel on stérilise l'ensemble de l'émulsion homogénéisée. 3. Method according to claim 1, wherein the whole of the homogenized emulsion is sterilized. 4. Procédé selon l'une des revendications 1 à 3, dans lequel le liquide stabilisateur, comporte une proportion d'atomes d'oxygène inférieure à 2 atomes pour 10 atomes de carbone. 25 4. Method according to one of claims 1 to 3, wherein the stabilizing liquid has a proportion of oxygen atoms of less than 2 atoms per 10 carbon atoms. 25 5. Procédé selon l'une des revendications 1 à 4, dans lequel on utilise, en plus du saponide émulsionnant, au moins un co-émulsionnant d'origine naturelle ou synthétique. 5. Method according to one of claims 1 to 4, wherein is used in addition to the emulsifying saponide, at least one co-emulsifier of natural or synthetic origin. 6. Emulsion aqueuse fabriquée selon le procédé de l'une des revendications 1 30 à 5 An aqueous emulsion made according to the process of one of claims 1 to 5 7. Gel comportant l'émulsion de la revendication 6 et un épaississant. 7. Gel comprising the emulsion of claim 6 and a thickener. 8. Crème comportant l'émulsion de la revendication 6 et un épaississant. 35 40 8. Cream comprising the emulsion of claim 6 and a thickener. 35 40
FR0902520A 2009-05-26 2009-05-26 Preparing aqueous emulsion of oily active substance, useful for e.g. cosmetic and food use, comprises mixing hydrophilic component (water and saponin emulsifier), mixing lipophilic components (substance and stabilizer) and homogenizing Pending FR2945936A1 (en)

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US20130344259A1 (en) * 2012-06-22 2013-12-26 Atlas Pearls And Perfumers Ltd Pearl treatment composition and method
WO2014101941A1 (en) * 2012-12-27 2014-07-03 Jean-Claude Epiphani Method for manufacturing an oil-in-water emulsion from an oily active substance, for cosmetic, food, or pharmaceutical use
EP3991714A1 (en) * 2020-10-28 2022-05-04 Amorepacific Corporation Nanoemulsion cosmetic composition and process for preparing same

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DATABASE CA [online] CHEMICAL ABSTRACTS SERVICE, COLUMBUS, OHIO, US; 26 May 1999 (1999-05-26), MATSUDA, HIDENORI ET AL: "Stable oil-in-water emulsions for cosmetics, food, and pharmaceuticals", XP002563769, retrieved from STN Database accession no. 1990:204453 *
DATABASE WPI Week 198407, Derwent World Patents Index; AN 1984-039607, XP002563894 *
DATABASE WPI Week 198934, Derwent World Patents Index; AN 1989-244468, XP002092980, "Oil-in-polyol and oil-in-water emulsions for cosmetics - prepd. by heating mixt. of hydrogenated lecithin, saponin and polyol then adding oil etc" *
VAN DE VEN ET AL: "High pressure versus heat treatments for pasteurisation and sterilisation of model emulsions", INNOVATIVE FOOD SCIENCE AND EMERGING TECHNOLOGIES, ELSEVIER, AMSTERDAM, NL, vol. 8, no. 2, 17 April 2007 (2007-04-17), pages 230 - 236, XP022032329, ISSN: 1466-8564 *

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WO2014101941A1 (en) * 2012-12-27 2014-07-03 Jean-Claude Epiphani Method for manufacturing an oil-in-water emulsion from an oily active substance, for cosmetic, food, or pharmaceutical use
US20150327566A1 (en) * 2012-12-27 2015-11-19 Jean-Claude Epiphani Method for manufacturing an oil-in-water emulsion from an oily active substance, for cosmetic, food, or pharmaceutical use
EP3708143A1 (en) * 2012-12-27 2020-09-16 Jean-Claude Epiphani Method for manufacturing an aqueous emulsion of an oily active substance for cosmetic, food or pharmaceutical use
US11000046B2 (en) 2012-12-27 2021-05-11 Jean-Claude Method for manufacturing an oil-in-water emulsion from an oily active substance, for cosmetic, food, or pharmaceutical use
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