EP3541182A1 - Stabile feste zusammensetzung auf der basis von aromatischen verbindungen und verwendungen davon - Google Patents

Stabile feste zusammensetzung auf der basis von aromatischen verbindungen und verwendungen davon

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Publication number
EP3541182A1
EP3541182A1 EP17828781.9A EP17828781A EP3541182A1 EP 3541182 A1 EP3541182 A1 EP 3541182A1 EP 17828781 A EP17828781 A EP 17828781A EP 3541182 A1 EP3541182 A1 EP 3541182A1
Authority
EP
European Patent Office
Prior art keywords
composition according
composition
acid
aromatic alcohol
caused
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.)
Withdrawn
Application number
EP17828781.9A
Other languages
English (en)
French (fr)
Inventor
Mounia OUKHOUIA
Chaimae Imane SENNOUNI
Hakima MOUSSA
Meryem MARZOUQ
Adnane Remmal
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.)
Individual
Original Assignee
Individual
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
Application filed by Individual filed Critical Individual
Publication of EP3541182A1 publication Critical patent/EP3541182A1/de
Withdrawn legal-status Critical Current

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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/12Powders or granules
    • A01N25/14Powders or granules wettable
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01CPLANTING; SOWING; FERTILISING
    • A01C1/00Apparatus, or methods of use thereof, for testing or treating seed, roots, or the like, prior to sowing or planting
    • A01C1/06Coating or dressing seed
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/34Shaped forms, e.g. sheets, not provided for in any other sub-group of this main group
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N3/00Preservation of plants or parts thereof, e.g. inhibiting evaporation, improvement of the appearance of leaves or protection against physical influences such as UV radiation using chemical compositions; Grafting wax
    • A01N3/02Keeping cut flowers fresh chemically
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    • A23B4/00General methods for preserving meat, sausages, fish or fish products
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    • A61K8/022Powders; Compacted Powders
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/19Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
    • A61K8/20Halogens; Compounds thereof
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
    • A61KPREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
    • A61K8/00Cosmetics or similar toiletry preparations
    • A61K8/18Cosmetics or similar toiletry preparations characterised by the composition
    • A61K8/30Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/34Alcohols
    • A61K8/345Alcohols containing more than one hydroxy group
    • AHUMAN NECESSITIES
    • A61MEDICAL OR VETERINARY SCIENCE; HYGIENE
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    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
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    • A61K8/33Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
    • A61K8/36Carboxylic acids; Salts or anhydrides thereof
    • A61K8/365Hydroxycarboxylic acids; Ketocarboxylic acids
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    • A61K8/72Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
    • A61K8/73Polysaccharides
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    • A61K8/97Cosmetics 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
    • A61K8/9783Angiosperms [Magnoliophyta]
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    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Definitions

  • the present invention relates to a stable composition based on natural or synthetic aromatic compound and its various uses, particularly in the agricultural field.
  • biopesticides based on plant extracts are also not suitable because of both their liquid form which makes the storage rather delicate because it requires a precise temperature and humidity, and both the risk of evaporation of the active ingredients.
  • biopesticides based on plant extracts several studies have focused on essential oils and their major compounds such as thymol, carvacrol and eugenol in particular (Koulo et al., 2008) Essential Oils as Green Pesticides: Potential and Constraints Biopestic 4 (1): 63-84, lsman, MB and Machial, CM (2006) .Pesticides basedon plant essential oils: from traditional practice tocommercialization.In M.
  • the object of the present invention is therefore to find a solution to these problems and to propose in particular a stable formulation comprising aromatic compounds of volatile nature having antimicrobial (antibacterial, antifungal, antiviral and antiparasitic) and / or anti-insect activity.
  • the subject of the invention is a composition in solid form, stable and dispersible in water, comprising:
  • At least one aromatic alcohol or at least one mixture containing it as an essential oil at least one aromatic alcohol or at least one mixture containing it as an essential oil
  • At least one emulsifying agent and / or an oil at least one emulsifying agent and / or an oil
  • At least one effervescent acid-base pair at least one effervescent acid-base pair.
  • Aromatic alcohols have many properties depending on their chemical formula, and the composition according to the invention can be advantageously used in particular as a phytosanitary product or fertilizer, but the composition according to the invention can also be used for other applications such as for example anti-insect or antimicrobial to sanitize ambient air, hands, buildings, reusable medical devices, etc.
  • FIG. 1 an image of the composition according to the invention of Example 1, before dispersion,
  • emulsifying agent within the meaning of the invention is meant any compound capable of improving the suspension and dispersion of a composition in water.
  • emulsifying agent when used in the singular in the present application, it means one or more emulsifying agents, the composition according to the invention may comprise one or more emulsifying agents.
  • texturing agent in the sense of the invention is meant any compound having the functions of stabilizer (improves stability), thickener (increases the viscosity) and / or emulsifier (improves the suspension).
  • texturizing agent when used in the singular in the present application, it means one or more texturing agents, the composition according to the invention may comprise one or more texturing agents.
  • aromatic alcohol means an aromatic molecule having an OH hydroxyl group attached to a carbon of a benzene ring.
  • Aromatic alcohol is also called phenol.
  • aromatic alcohol may be used interchangeably in the singular or the plural in the present application. Whether used singular or plural, it is always necessary to hear at least one aromatic alcohol that is to say one or more aromatic alcohols, the composition according to the invention may comprise one or more aromatic alcohols.
  • anti-insect in the sense of the invention is meant any inhibitory action and / or destructive insects and pests.
  • antimicrobial in the sense of the invention is meant any inhibitory action and / or destructive bacterial, fungal, parasitic and viral.
  • compound in the sense of the invention is meant a molecule or a mixture of molecules.
  • acid-base effervescent pair means the combination, the combination of an acid and a base capable of causing an effervescent phenomenon when said pair is put in solution.
  • acid-base pair effervescent when used in the singular in the present application, it means one or more acid-base pairs, the composition according to the invention may comprise one or more acid-base pairs.
  • dispenser in water in the sense of the invention is meant capable of dispersing, of solubilizing in water without forming non-dispersible masses, especially in the sprinkler irrigation water of plants or watering animals
  • essential oil within the meaning of the invention is meant any extract obtained from one or more aromatic plant (s), preferably the concentrated and hydrophobic liquid volatile aromatic compounds (odérisings) of a plant.
  • An essential oil may in particular be obtained by mechanical extraction and steam distillation or by dry distillation.
  • essential oil is also meant products identical to those described above but obtained by chemical synthesis.
  • mixture containing an aromatic alcohol within the meaning of the invention means any mixture of molecules comprising at least one aromatic alcohol. It may be preferentially one or more essential oil (s) or one or more mixture (s) of molecules contained in one or more essential oil (s) or a mixture of one or more essential oils with one or more mixture (s) of molecules contained in one or more essential oils.
  • mixture containing an aromatic alcohol means one or more mixtures containing an alcohol aromatic composition
  • the composition according to the invention may comprise one or more mixtures containing an aromatic alcohol.
  • stable product within the meaning of the invention means a product whose molecular composition and texture, color and efficiency are constant over time.
  • solid means a non-liquid form that is preferably uniform: powder, pellet or tablet.
  • the invention therefore relates to a composition in solid form, stable and dispersible in water.
  • composition according to the invention may especially be in the form of powder, pellets or tablets.
  • composition according to the invention comprises at least one aromatic alcohol or at least one mixture containing at least one aromatic alcohol.
  • Said at least one aromatic alcohol is a natural or synthetic aromatic alcohol.
  • said at least one aromatic alcohol is mono, di or sesquiterpeniques. It may in particular be chosen from thymol, menthol, eugenol, carvacrol and cinnamaldehyde.
  • the composition comprises at least one aromatic alcohol contained in an essential oil, and preferably the composition according to the invention comprises at least one essential oil, such as for example the essential oil of thyme, oregano , clove, mint.
  • Said at least one aromatic alcohol and / or said at least one mixture comprising at least one aromatic alcohol, present in the composition according to the invention play a role of active principle. They have effects and efficiencies that vary according to their nature, but they preferably have antibacterial and / or anti-insect activity, as is the case in particular aromatic alcohols chosen from thymol, menthol, eugenol, carvacrol and cinnamaldehyde.
  • the aromatic alcohol or the mixture comprising at least one aromatic alcohol represents between 0.1 and 25% by weight of the composition.
  • the composition according to the invention also comprises at least one emulsifying agent and / or an oil.
  • the emulsifying agent and / or the oil are preferably chosen from vegetable oils, mineral oils, soy lecithin, cellulose, pectin and glycerol.
  • Said at least one emulsifying agent and / or oil makes it possible in particular to liquefy and / or maintain in suspension the aromatic alcohol when it is dissolved. Indeed ; Emulsifiers and / or oils interact with both aromatic alcohol molecules and water molecules, which prevents aromatic alcohol molecules from floating on the surface of the water.
  • the emulsifying agent and / or the oil represents between 0.01 and 2% by weight of the composition.
  • composition according to the invention in addition to these first two constituents, also comprises at least one texturing agent. It is preferably chosen from locust bean gum, guar gum and cassia gum.
  • Said at least one texturing agent makes it possible in particular to improve the stabilization of the aromatic alcohols present in the composition both during storage and during dissolution.
  • the texturing agent allows, at the time of manufacture, to set the aromatic alcohols and emulsifiers and / or oils that are liquid and therefore to obtain a sieving powder.
  • the volatile aromatic alcohols remain fixed on the texturizing agents and do not evaporate.
  • the texturizing agents create a viscosity that promotes the dispersion of aromatic alcohols and prevents them from floating.
  • said at least one texturing agent represents between 5 and 12% by weight of the composition.
  • the ratio of the gum must not exceed 12%, preferably 10%, in the final composition, if not once in solution, the texturing agent may form a paste difficult to disperse.
  • the composition according to the invention also comprises at least one effervescent acid-base pair. It is preferentially chosen from the following acid-base pairs: sodium bicarbonate-citric acid, calcium bicarbonate-citric acid, potassium bicarbonate-citric acid, sodium bicarbonate-tartaric acid, calcium bicarbonate-tartaric acid, potassium bicarbonate - tartaric acid, sodium bicarbonate-maleic acid, sodium bicarbonate-maleic acid, potassium bicarbonate-maleic acid, sodium bicarbonate-ascorbic acid, calcium bicarbonate-ascorbic acid and potassium bicarbonate-ascorbic acid.
  • the couple's acid effervescent represents between 20 and 25% by weight of the composition and the base of the effervescent couple represents between 60 and 74.89% by weight of the composition.
  • Said at least one effervescent acid-base pair present in the composition in particular makes it possible to improve the dissolution of the aromatic alcohol once in solution.
  • said at least one effervescent acid-base pair represents between 50 and 94.89% by weight of the composition.
  • composition according to the invention consists exclusively of:
  • emulsifying agent s
  • oil s
  • one or more effervescent acid-base couple (s).
  • composition according to this variant may in particular be constituted as follows:
  • the aromatic alcohol (s) or the mixture (s) of aromatic alcohol (s) represent (s) between 0.1 and 25% by weight of the composition
  • the emulsifying agent (s) and / or the oil (s) represent (s) between 0.01 and 2% by weight of the composition
  • the texturizing agent (s) represents (s) between 5 and 12% by weight of the composition
  • the effervescent acid-base pair (s) represent (s) between 61 and 94.89% by weight of the composition.
  • the composition according to the invention comprises at least one other compound, such as for example at least one compound chosen from vitamins, minerals, hormones, dyes, etc.
  • composition according to the invention can be obtained by any suitable method for obtaining a composition in solid form with the aforementioned constituents.
  • stirring in particular in a tank with agitator rotating between 30 and 120 revolutions per minute, preferably for 5 to 45 minutes, at a temperature of between 40 and 60 ° C., and / or
  • This first step makes it possible to obtain a good dissolution of the aromatic alcohols, without any problem of recrystallization.
  • the solution is then added to a powder containing at least one texturing agent and an effervescent acid-base pair, preferably under the following conditions:
  • stirring in particular in a mixer / mixer, still more preferably for 10 to 40 minutes, and / or
  • the texturing agent makes it possible to stabilize the volatile molecules by absorption in the final composition.
  • the effervescent acid-base pair improves the dissolution of the composition which can be carried out without necessarily resorting to manual or mechanical agitation.
  • the initial powder consisting of the texturizing agent and the acid-base pair progressively absorbs the liquid consisting of the aromatic alcohol and the emulsifying agent and / or oil until a powder sometimes containing small lumps. These little lumps are converted into powder by the action of the calibrator; the calibration is done after the powder has been removed from the mixer. (The final powder obtained after calibration is preferably stored in hermetically sealed bags away from heat and humidity at room temperature).
  • the composition according to the invention can be used for different applications.
  • the solid composition according to the invention is preferably dissolved.
  • the composition / water ratio is between 100g per 1000 liters of water up to 25 kg per 1000 liters of water.
  • the aromatic alcohols have antibacterial and / or antifungal and / or antiviral and / or anti-insect properties.
  • the invention therefore aims in particular at using a composition according to the invention as a phytosanitary product, in particular for preventing and / or controlling plant diseases (all or part of the plants) caused by fungi, bacteria, bacteria viruses, nematodes and / or pests.
  • composition according to the invention can be used in irrigation water or leaf sprinkling.
  • Plant diseases caused by bacteria for which the composition according to the invention is particularly useful in prevention and / or treatment are preferably chosen from soft rot caused by Erwinia species, bacterial canker caused by Pseudomonas species or gall. snout caused by Agrobacterium species.
  • the plant diseases caused by fungi for which the composition according to the invention is particularly useful in prevention and / or treatment are preferably chosen from Fusarium wilt caused by Fusarium species, late blight caused by Phytophthora species, powdery mildew caused by fungi. by the species Podosphaera and Oidium, Alternaria caused by Alternaria species, sooty mold caused by Alternaria and Cladosporium species, or Botrytis gray mold.
  • the pests causing plant diseases against which the composition according to the invention is particularly useful in prevention and / or treatment are chosen from aphids, midges, soil mites or noctuids.
  • composition according to the invention can be used specifically to prevent and / or fight against post-harvest diseases of fruits, vegetables and / or flowers caused by fungi, bacteria, viruses, nematodes and / or pests. .
  • the composition according to the invention can be used to prevent and / or fight against citrus rot caused by Penicillium and Geotrichum species, or to prevent and / or fight against the fungal deterioration of dates caused by Aspergillus species.
  • composition according to the invention can also be used for antifungal treatment during the coating of seeds, in particular seeds selected from wheat, barley, lentils, chickpeas and beans.
  • composition according to the invention can be used as a phytosanitary product for:
  • composition according to the invention can also advantageously be used to stimulate plant growth, in particular to stimulate rhizogenesis in plants.
  • composition according to the invention can be used directly on objects, floors, walls, etc., in particular for:
  • composition according to the invention can also be used as a bath for decontaminating animal carcasses in slaughterhouses or for decontaminating poultry eggs before placing them in incubators.
  • composition according to the invention is particularly effective and can be used to disinfect reusable medical devices, in particular fibroscopes, colonoscopes, bronchoscopes and sinuscopes.
  • reusable medical devices in particular fibroscopes, colonoscopes, bronchoscopes and sinuscopes.
  • the composition can also be used:
  • the composition according to the invention can therefore be used for many applications. It has the advantage of being in solid and stable form which allows long-term storage of at least two years and easy and economical transportation. In addition, the composition is very easily dispersible in water, which allows an easy and economical use in solution.
  • compositions according to the invention uses and test results demonstrating their effectiveness.
  • Example 1 The composition of Example 1 consists of:
  • Example 2 The composition of Example 2 consists of:
  • This composition is obtained by the implementation of the following steps: 15 g of menthol are preheated to 50 ° C and mixed with 0.2 ml of mineral oil, then the mixture is added to the combination 10 g of guar gum, 50.54 g of potassium bicarbonate and 24.26 g of tartaric acid. The whole is suspended in 10 l of water.
  • Example 3 The composition of Example 3 consists of:
  • Example 4 The composition of Example 4 consists of:
  • Aromatic alcohols do not readily disperse in water due to their hydrophobic nature.
  • the prior art proposes a method for dispersing these compounds by the addition of a surfactant and a solvent (WO2009124392A1), but this method is not suitable because it is known that surfactants and solvents decrease the activity of phenolic compounds (Remmal A., Bouchikhi T., Tantaoui-Elaraki A., Ettayebi M. (1993) Inhibition of antibacterial activity of essential oils by Tween 80 and ethanol in liquid medium J. Pharm. 352-356).
  • certain aromatic alcohols such as thymol or menthol, are in crystallized form at room temperature and once in contact with water, if one tries to make them liquid by heating them, they recrystallize.
  • composition according to the invention associating the aromatic alcohols with a texturizing agent, an emulsifying agent (and / or an oil) and an effervescent acid-base pair makes it possible at the same time to prevent the recrystallization of the aromatic alcohols in crystallized form, from ensure the stability of the aromatic alcohols and the composition, its homogeneity and facilitate its dispersion during its dissolution.
  • the shape and dispersion in water of the composition of Example 1 was evaluated in comparison with other compositions comprising an aromatic alcohol alone or with only one or more other constituents of the composition according to the invention.
  • composition Cl consists of 15% of Thymol only.
  • This composition is obtained by suspending 15 g of Thymol in 10 l of water.
  • composition C2 constituted by:
  • composition C3 constituted by:
  • the mixture is then added to the combination of sodium bicarbonate and citric acid,
  • composition C4 constituted by:
  • Example 1 In order to evaluate the effectiveness of the composition according to the invention (Example 1). It has been tested in vitro on several strains of bacteria, yeasts and mold causing disease and damage in plants.
  • strains tested in this study were isolated, purified and identified.
  • 11 strains of fungal origin including 5 of the genus Fusarium, one of the genus Penicillium, one of the genus Geotrichum, one of the genus Alternaria, one of the genus Sclerotonia and the last of the genus Helminthosporium.
  • Two strains of yeast origin one of the genus Candida and the other of the genus Saccharomyces. The two remaining strains are of bacterial origin.
  • the culture media used are: Sabouraud dextrose agar and broth (Biokar) for the cultivation and testing of the antifungal activity of fungal strains.
  • the culture media were prepared according to the instructions of the supplier, different concentrations of the composition were used to determine the MIC (minimum inhibitory concentration) in an agar medium and in a liquid medium, the CMF (minimum fungicidal concentration) in a liquid medium. using the macrodilution technique.
  • agar medium In flasks containing 60 ml of the appropriate medium, autoclaved for 20 minutes at 121 ° C. and cooled to 45 ° C., different amounts of the composition of Example 1 are added, making it possible to obtain the final concentrations: (0.41, 0.82, 1.65, 3.33, 6.67, 13.34, 26.68 and 53.36 g / l). Negative controls containing the medium alone are also prepared, the flasks are then poured into petri dishes (90 ⁇ 16 mm) and allowed to cool at 4 ° C. for 24 hours, then inoculated with a volume of 10 .mu.l of a stock suspension. 10 6 spores / ml of the appropriate mold. After diffusion of the deposited drop, the dishes are incubated at 27 ° C. for 5 days. The test is carried out in triplicate and repeated three times.
  • liquid medium Sabouraud culture broth sterilized by autoclaving for 20 min at 121 ° C and cooled to room temperature was dispensed into sterile test tubes. Then, increasing concentrations of the composition according to the invention of: (0.41, 0.82, 1.65, 3.33, 6.67, 13.34, 26.68 and 53.36 g / l) have been tested. All the tubes were inoculated with 20 ⁇ l of the mother suspension of spores (10 6 spores / ml). The final concentration in each tube is calculated for a final volume of 5ml. The tubes are thus incubated at 27 ° C. with stirring at 130 rpm for 5 days.
  • CMF Comparative Mortality Figure
  • the test of the antibacterial activity of the composition according to the invention was carried out following the same procedure as that carried out in the test of the antifungal activity except that the culture medium used for this test is Mueller Hinton (agar and broth). ), the inoculum of bacteria inoculated is of the order of 10 7 bacteria / ml and the incubation temperature is of the order of 37 ° C.
  • Tobleou 2 Thieves of MIC and CMF of the composition according to the invention for fungal species
  • composition proved very effective against the fungal species used in this test.
  • MIC and CMB values obtained with the composition of Example 1 in the test of antifungal activity on bacterial species are presented in Table 3.
  • Example 1 In order to evaluate the effectiveness of the composition according to the invention of Example 1, it has been tested in vitro or in vivo on several insects, parasites and nematodes.
  • Macrosiphum rosae (rose-flowering aphid) were removed using a fine brush and brought into contact with different doses of the composition according to the invention.
  • a paper towel absorbent soaked with solutions containing increasing doses of the composition according to the invention (1.67; 3,33; 6,67 and 13,34 g / 1).
  • Petri dishes served as controls containing normal water. 20 adults were put in each box, the experiment was established in triplicate.
  • Example 1 the in vivo efficacy of the composition according to the invention (Example 1) was tested on the species Rhizoglyphus callae (soil mite) in their usual medium which is soil.
  • Rhizoglyphus callae soil mite
  • flower pots freesia
  • solutions containing increasing doses of the composition according to the invention (1 67, 3.33, 6.67 and 13.34 g / l).
  • Control pots received only water as irrigation solution, the experiment was repeated three times. After a few hours of contact with the irrigation solution, a few grams of soil from each pot were taken and suspended in water, an observation and a binocular magnifying glass count were made to determine the percentage. mortality for each dose used in this test.
  • composition according to the invention was also tested in vitro on nematodes and more specifically the species Heterodera spp from an infected soil (previously treated with different concentrations of the composition of Example 1).
  • the method used is that of Baerrman. It is a method of separating nematodes from soil particles according to their sizes and weights according to the following steps:
  • the nematodes thus counted are brought into contact with different doses of the composition according to the invention.
  • the dilutions used are:
  • Nt and Nm respectively represent the total number of insects and the number of dead insects. The results are shown in Table 4.
  • composition according to the invention generates a very powerful insecticidal effect.
  • the dose of 6.67 g / 1 was lethal for aphids and nematodes while the 3.33 g / 1 dose was effective against soil mites after only a few hours of contact.
  • composition according to the invention (Example 1) was tested in vivo on Fusarium vascular wilt caused by Fusgrium oxysporum sp dignthi. Eight seedlings per lot of the Martina variety were used in this test.
  • Fusarium spores (10 6 spores / ml) were inoculated into the siliceous sand near the roots of each plant.
  • PNINT Uninfected, untreated plants.
  • PIT 3.33 g / l Infected plants treated with 3.3 g / l of the composition according to the invention.
  • PIT 6.67 g / l Infected plants treated with 6.67 g / l of the composition according to the invention.
  • PIT 13.34 g / l Infected plants treated with 13.34 g / l of the composition according to the invention.
  • the dilutions used are:
  • the mode of application is an irrigation application.
  • Tobleou 6 Effect of the composition according to the invention on the growth of carnations infected by fusimiosis.
  • the 13.34 g / l dose was found to be too high for carnations, since it generated a phytotoxic effect on the aerial part and even on the root system of the plant.
  • composition in the irrigation water thus makes it possible to reduce the fungal load of the soil. This will have a positive impact on the health and well-being of the young plant that will develop.
  • Example 1 The stimulating effect of the growth of the composition according to the invention (Example 1) was also tested on carnation seedlings of the West diamond variety.
  • PT 1 g / 1 Plants treated with 1 g / 1 of the composition according to the invention.
  • PT 1.65 g / 1 Plants treated with 1.65 g / 1 of the composition according to the invention.
  • PT 3.33 g / 1 Plants treated with 3.33 g / 1 of the composition according to the invention.
  • the stimulating effect of the composition according to the invention was quantified by taking measurements of the agromorphological characters (the number of shoots, the distance between nodes, the number of nodes, the length of the stem, the diameter of stem and number of flower buds) after three months of treatment with three applications per week in irrigation water.
  • the dilutions used are:
  • the mode of application is by irrigation.
  • Table 7 Stimulating effect of the growth of the composition according to the invention on carnation seedlings
  • Example 1 The stimulating effect of the composition according to the invention (Example 1) was tested on seedlings of date palms resulting from the germination of date kernels of the Mejhoul variety.
  • One-leaf seedlings received different doses of the composition of Example 1 according to the invention (0; 1.65; 3.33; 6.67 g / l).
  • the seedlings were harvested and the fresh and dry weight of the root portion of each seedling was determined.
  • the dilutions used are:
  • the mode of application is by irrigation.
  • Table 8 Stimulating effect of the rhizogenesis of the composition according to the invention in date palm seedlings
  • a swab sample of eight dates from each box was taken.
  • the sampling area is 1 cm 2 per date.
  • the dilutions used are:
  • the mode of application is by soaking.
  • Table 9 Bacterial load contained in the dates treated with the composition according to the invention and those not treated (cfu / cm 2 )
  • Tables 9 and 10 respectively show the results of the bacterial load and the fungal load contained in the processed and untreated dates.
  • the 6.67 g / l dose was found to be the most effective since the dates soaked in this dose remain free of bacteria and fungi that can affect their storage for one month at room temperature.
  • composition according to the invention (Example 1) was also tested on the vase performance of cut flowers and more specifically carnations. To do this the carnation flowers were cut and equalized to 55 cm in length before being soaked in solutions containing two concentrations of the composition according to the invention (1.6 and 3.3 g / 1) immediately after harvesting.
  • the dilutions used are:
  • the mode of application is as follows: setting in vase.
  • composition according to the invention improves the vase performance of the cut flowers.
  • Example 1 The effectiveness of the composition according to the invention (Example 1) was tested on the microbial load (bacteria, yeasts and molds, parasites) of water used in watering poultry. The sample is transported to the laboratory and kept cool for the in vitro test.
  • microbial load bacteria, yeasts and molds, parasites
  • the culture media used are:
  • PCA Plate Count Agar
  • TSC Teryptone Sulphite Cycloserine Agar (Biokar) for cultivation and testing of antibacterial activity of anaerobic bacteria.
  • Wilson-blair agar (Biokar) for culture and testing of the antibacterial activity of salmonella.
  • the antibacterial activity test of the composition according to the invention was carried out as follows:
  • Example 1 Different concentrations of the composition of Example 1 (1 g / l, 2 g / l, 4 g / l) were added to the water sample. A negative control containing the water alone sample is also prepared.
  • the culture media were prepared according to the supplier's instructions, sterilized by autoclaving for 15 minutes at 121 ° C and cooled to 45 ° C. They were then poured into petri dishes (90 ⁇ 16 mm) and allowed to cool at 4 ° C for 24 hours and then inoculated with a volume of 100 ⁇ of the water sample. The plates are incubated at 37 ° C for 24h for revivable, total compliant aerobic bacteria, salmonella, staphylococci and anaerobic bacteria. For faecal conforms, the dishes are incubated at 44 ° C. for 24 hours.
  • the test of the antifungal activity of the composition according to the invention was carried out following the same protocol as that carried out in the antibacterial activity test, except that the incubation temperature is of the order of 27.degree. the incubation time is 3 to 5 days.
  • the pest control activity test a volume of ⁇ of water sample was placed between a glass slide and the Malassez cell. The number of cells in 10 rectangles was then counted.
  • composition according to the invention has also been tested in vivo on chicks. Twelve chicks per batch were used in this test. Throughout the test period, the temperature of the facility was adjusted to 28 ° C and the animals had free access to the water and feed that was available continuously.
  • the water used in this test is the surface water taken from the drinking water distribution tank that was used in the in vitro test.
  • each batch of chicks is weighed from the first day. Then, individual weighings are performed at the end of each phase. Average live weight is determined as follows:
  • Mean live weight (g) Weight of all chicks in a batch / Number of chicks in this batch
  • the gain in live weight the chicks of each batch were weighed on arrival for the calculation of average weight at startup. Subsequently, the weighings were carried out at the end of each rearing phase until the end of the experiment.
  • the weight gain is determined by the following formula:
  • the live weight gain (g) P2 - PI
  • the consumption index (IC) corresponds to the quantity of food necessary to produce 1 kilogram of live weight.
  • the IC is determined for each phase by the following formula:
  • IC Quantity of food consumed during a phase
  • Mortality rate mortality is recorded daily. The mortality rate is determined for each batch during a given phase by the following formula:
  • Mortality rate (%) number of dead chicks during a phase x 100
  • Tobleou 14 Effect of the composition according to the invention on the average live weight and the average weight gain
  • composition according to the invention on reducing the intestinal load of animals (broiler chicks)
  • Example 1 The effect of the composition according to the invention (Example 1) was tested on reducing the intestinal load (revivable aerobic bacteria and parasite load) of the broiler chicks for 35 days. Every 7 days, droppings samples from the different batches were taken and solubilized in physiological saline (1 g of droppings in 9 ml of physiological saline).
  • the culture medium used is:
  • PCA Platinum Count Agar
  • Biokar PCA (Plate Count Agar) for the culture of revivable aerobic bacteria.
  • the culture medium was prepared according to the instructions of the supplier, sterilized by autoclaving for 15 minutes at 121 ° C. and cooled to 45 ° C., then poured into Petri dishes (90 to 16 mm) and allowed to cool. at 4 ° C for 24 hours, then inoculated with a volume of 100 ⁇ of the sample. The dishes are incubated at 37 ° C. for 24 hours. The test is performed in triplicate.
  • Tobleou 16 Effect of the composition according to the invention on the reduction of the intestinal charge in revivable aerobic bacteria
  • Second sampling carried out under the same conditions and respecting the same steps as during the first sampling.
  • Tobleou 19 Action ontibocterian between the two products tested.
  • the results obtained detected the presence of a bacterial carpet before disinfection; the same result was obtained after disinfection with glutaraldehyde, whereas after disinfection by the composition according to the invention, the bacterial load was only 50 CFU / ml with the concentration 1/1000 and zero with the concentration 1/500.
  • composition according to the invention on post-harvest fruit treatment of clementines (variety "Afourar") Drencher and Waxing. Fruits infected experimentally by spore injection
  • Lot 1 contains 10 fruits, washed with a slurry consisting of chemical fungicides (Imazalil at a dose of 500cc / hl and Orthophenylphenol at a dose of 750 ppm).
  • chemical fungicides Imazalil at a dose of 500cc / hl and Orthophenylphenol at a dose of 750 ppm.
  • Lot 2 contains 10 fruits, washed with a slurry constituted by the composition according to the invention at a dose of 3kg per ton of water.
  • Lot 3 contains 10 fruits, waxed by a mixture of wax and imazalil at a dose of 3000ppm, then dried with hot air (50 ° C).
  • Lot 4 contains 10 fruits, waxed with a mixture of wax and the composition according to the invention at a dose of 10 kg per ton, and then dried (50 ° C.).
  • Lot 5 contains 10 fruits washed by a slurry consisting of chemical fungicides (Imazalil at a dose of 500cc / hl and Orthophenylphenol at a dose of 750 ppm), after drying they were waxed with a mixture of wax and the imazalil at a dose of 3000ppm, and then dried (50 ° C).
  • chemical fungicides Imazalil at a dose of 500cc / hl and Orthophenylphenol at a dose of 750 ppm
  • Lot 6 contains 10 fruits washed with a slurry constituted by the composition according to the invention at a dose of 3 kg per ton of water, after drying they were waxed with a mixture of the wax and the composition according to the invention at a dose of 10kg per ton, then dried (50 ° C).
  • the washing was carried out using a hand shower that allows the fruits to be washed in a manner comparable to that of the Drencher in the packing station.
  • the waxing was applied by nebulisation in a manner comparable to that of a waxing system in the packing station.
  • each fruit of the six lots was infected by injection of a volume of 100 ⁇ l of a suspension of spores of the strain Penicillium digitatum (10 6 spores / ml), using a syringe equipped with a very fine needle (30 gauges), so inclined tangential to the surface of the albedo.
  • the injection site is marked by a circle marked with an indelible marker.
  • the fruits were then incubated at a temperature of 20 ° C.
  • results obtained show that the rot starts from the third day after the infection in the batch washed with the chemical fungicides, whereas in batch washed with the composition according to the invention the rot only begins after four days.
  • results also show that the decay in the batch washed with the chemical fungicides develops more rapidly with a diameter of 3.2 cm ⁇ 0.7 after 7 days, compared to the batch washed with the composition according to the invention where the diameter rot only reaches 2 cm ⁇ 0.6 after 7 days.
  • results also show a delay in the appearance of spores in the batch treated with the composition according to the invention in comparison with the batch treated with chemical fungicides.
  • the preparation of the invention provides better protection than chemical fungicides when used for washing and waxing fruit experimentally infected with an extreme number of spores located in the injection site.
  • Lot 2 10 fruits washed with a slurry constituted by the composition according to the invention at a dose of 3 kg per ton of water, then waxed with a mixture of wax plus the preparation of the invention at a dose of 10 kg per ton then dried at 50 ° C
  • Tobleou 20 Percentage of the surface rots on fruits treated with the composition of the invention compared to fruits treated with imazalil and untreated fruits:
  • composition according to the invention allows preservation of fruit for 12 days without rotting while for the group treated with chemical fungicides rot appeared in the 6 th day. For lot without treatment, rot appeared in the 4 th day.
  • Field trials were conducted on a citrus farm. In these tests, a batch of four cases of fruit of the variety "Afourar” soaked directly after their picking in the water containing the preparation of the invention at a dose of 1 kg per ton, another batch of 4 cases of fruit dipped directly after picking in water alone. 30 fruits were taken from each lot, and the fungal load of each fruit was evaluated as a number of spores (colony-forming units) per square centimeter of fruit surface.
  • results obtained show that the fungal load of fruits soaked in a solution with the composition according to the invention is of the order of 10 5 spores per cm 2 , lower than the fungal load of fruits soaked in water alone which reaches 10 8 spores per cm 2 .
  • results show that the fruits soaked in the preparation of the invention will arrive at the packing station with a lower initial load (1000 times lower) than that of the fruits soaked in water alone.
  • Tobleou 21 Fruit fungal load treated with the composition according to the invention or with chemical fungicides in the drencher step and the waxing step. Load expressed as number of spores (CFU / cm2) per cm2
  • results obtained show that there is a significant difference in the fungal load of the fruits treated with the composition according to the invention which is a thousand times lower than that of the fruits treated with the chemical fungicides after the drencher step and after step of waxing.
  • a second batch of 6 tons of fruits of the variety "Afourar" (batch composition) was washed with a slurry containing the water and the composition according to the invention at the dose of 3 kg per ton, and waxed with a mixture of the wax and the composition according to the invention at the dose of 5 kg per ton.
  • two sub-lots of 15 crates were taken from each lot and distributed as follows:
  • Sub-batch a 15 boxes of the Imazalil lot, stored at 8 ° C.
  • Sub-batch b 15 cases of the composition batch stored at 8 ° C.
  • sub batch c 15 boxes of the Imazalil lot stored at 25 ° C.
  • Sub-batch d 15 cases of the batch composition stored at 25 ° C. Sub lots were checked once a week for one month. Counting the rotten fruit in each batch reveals the evolution of the decay rate as a function of the storage temperature and the treatment used.
  • results obtained show that the rate of rotting in sub-batches preserved at a temperature of 25 ° C is higher compared to sub-batches kept at a temperature of 4 ° C.
  • results also show that the fruits treated with the composition according to the invention have a decay rate between 0.5% and 2.82% at a temperature of 4 ° C. and between 4.5% and 6.91% at 25 ° C. ° C, this rate is lower compared to the decay rate in fruits treated with chemical fungicides, which varies between 1.35% and 4.67% at a storage temperature of 4 ° C, and between 4.62% % and 9.68% at a temperature of 25 ° C.
  • Tests were carried out in a citrus packing station. In these tests, the ambient air of different areas of the station was sprayed with the preparation of the invention at a dose of 10 kg per ton of water twice a day; between 12 pm and 1 pm and at 6 pm Air samples (petri dish with PDA medium opened for 5 minutes) were made to evaluate the fungal load of the ambient air of each zone of the station before and after treatment and this four times a day:
  • Tobleou 23 number of colonies per petri dish
  • the growth rate of the three strains is monitored daily by measuring the diameter of the colonies.
  • Table 24 Evolution of the thallus diameter of the three strains cultivated in the presence of different concentrations of the composition according to the invention
  • composition according to the invention exerts a very strong partial inhibition on the three strains studied at the concentration of 0.75 g / l which corresponds to a treatment with 0.75 kg per ton of the composition. From the 1.25 concentration, there is complete inhibition on the three strains studied.
  • composition according to the invention has a very high efficacy against the main fungi responsible for citrus rot in post-harvest.
  • Lot 1 containing 120 tomatoes washed with a slurry containing the water and the composition according to the invention at a dose of 0.5 g / l.
  • a sub-lot has: 60 tomatoes from lot 1, stored at 25 ° C
  • a sub-lot d 60 tomatoes of lot 1, stored at 8 ° C Tomatoes from each sub-lot were monitored daily, and the percentage of dehydrated tomatoes was noted.
  • Table 25 Percentage of rotten cherry tomatoes in the batch washed with the composition of the invention, in comparison with the batch washed with chlorine, depending on storage conditions
  • results obtained show that the percentage of dehydrated tomatoes in sublots kept at a temperature of 25 ° C is higher compared to sub-batches kept at a temperature of 8 ° C.
  • results also show that the batch treated with the composition according to the invention has a lower percentage of dehydrated tomatoes compared to the dehydrated tomato level in the batch treated with chlorine.
  • Lot 1 containing 20 cherry tomatoes washed the composition according to the invention at a dose of 0.5 g / l.
  • Lot 3 containing 20 cherry tomatoes washed with water alone (Witness). After treatment, the tomatoes of each batch were wounded in the peduncle by a fine syringe (22G xl 1 ⁇ 4 "), and kept at a temperature of 27 ° C.
  • Tomatoes were monitored daily, and the percentage of tomatoes that showed peduncle rot was noted.
  • Tobleou 26 Percentage of cherry tomatoes that show peduncle rot depending on the treatment used

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EP17828781.9A 2016-11-18 2017-11-17 Stabile feste zusammensetzung auf der basis von aromatischen verbindungen und verwendungen davon Withdrawn EP3541182A1 (de)

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Application Number Priority Date Filing Date Title
FR1670691A FR3058871A1 (fr) 2016-11-18 2016-11-18 Composition stable solide a base de compose aromatique et utilisations
PCT/IB2017/057198 WO2018092075A1 (fr) 2016-11-18 2017-11-17 Composition stable solide a base de compose aromatique et utilisations

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US (1) US20190327961A1 (de)
EP (1) EP3541182A1 (de)
FR (1) FR3058871A1 (de)
MA (1) MA46922A (de)
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ZA (1) ZA201902996B (de)

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US11213469B1 (en) * 2017-07-07 2022-01-04 Michael Nghiem Le Effervescent foot bath and method
JP7463294B2 (ja) 2018-06-04 2024-04-08 ユニリーバー・アイピー・ホールディングス・ベスローテン・ヴェンノーツハップ 保存組成物
JP7374927B2 (ja) 2018-06-04 2023-11-07 ユニリーバー・アイピー・ホールディングス・ベスローテン・ヴェンノーツハップ 保存組成物
CN112154012B (zh) 2018-06-04 2023-10-03 联合利华知识产权控股有限公司 防腐组合物

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ZA201902996B (en) 2021-05-26
FR3058871A1 (fr) 2018-05-25
MA46922A (fr) 2019-09-25
WO2018092075A1 (fr) 2018-05-24
US20190327961A1 (en) 2019-10-31

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