WO2015071433A1 - Composition comprenant des capsules gélifiées stabilisées par un tampon - Google Patents
Composition comprenant des capsules gélifiées stabilisées par un tampon Download PDFInfo
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- WO2015071433A1 WO2015071433A1 PCT/EP2014/074663 EP2014074663W WO2015071433A1 WO 2015071433 A1 WO2015071433 A1 WO 2015071433A1 EP 2014074663 W EP2014074663 W EP 2014074663W WO 2015071433 A1 WO2015071433 A1 WO 2015071433A1
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- composition
- capsules
- gelled
- buffer
- polyelectrolyte
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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
- A61K8/11—Encapsulated compositions
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/19—Cosmetics or similar toiletry preparations characterised by the composition containing inorganic ingredients
- A61K8/20—Halogens; Compounds 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
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/49—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds
- A61K8/494—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing heterocyclic compounds with more than one nitrogen as the only hetero atom
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/55—Phosphorus compounds
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/733—Alginic acid; Salts thereof
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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
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/92—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof
- A61K8/922—Oils, fats or waxes; Derivatives thereof, e.g. hydrogenation products thereof of vegetable origin
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- 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
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- 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
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
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- 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
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5089—Processes
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- 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
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- 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
- A61K2800/80—Process related aspects concerning the preparation of the cosmetic composition or the storage or application thereof
- A61K2800/805—Corresponding aspects not provided for by any of codes A61K2800/81 - A61K2800/95
Definitions
- composition comprising gelled capsules
- the present invention relates to a composition comprising gelled capsules.
- Capsules with a simple or complex structure, with a polyelectrolyte membrane in the gelled state are known. These capsules are increasingly used in the fields of cosmetics and agri-food for their ease of implementation and their naturalness. Indeed, the membrane is composed of natural polyelectrolytes, such as alginate, a polysaccharide extracted from brown algae, laminaria.
- gelled capsules of alginate, carrageenan, gellan, and pectin are known.
- the principle of the formation of the membranes of these capsules is based on the gelation of the polyelectrolyte in the presence of divalent cations, such as, for example, Ca 2+ or Ba 2+ cations.
- divalent cations such as, for example, Ca 2+ or Ba 2+ cations.
- the alginate chains are composed of two types of monomers randomly chained to form the polymer chains: manuronate (M) and guluronate (G).
- M manuronate
- G guluronate
- the monomers G of 2 isolated chains can assemble to form a cage in which divalent cations can be inserted and chelated. Chelating bonds are then obtained between 2 initially isolated chains, which will serve as a crosslinking link and lead to the gelation of the alginate chain network, thus forming a solid membrane.
- the gelling principle is similar in the case of carrageenan, gellan or pectin.
- Such capsules can be produced using millifluidic, which allows complex structures of liquid drops to be created in another liquid, all of which is surrounded by a polyelectrolyte membrane to give the system strength and mechanical strength, after gelling. .
- the polyelectrolyte in the gelled state is in thermodynamic equilibrium between the chelated and gelled form, and the isolated and liquid form in solution. Any addition of charged molecules can thus disturb this equilibrium by creating new possible chelation sites for divalent cations.
- the polyelectrolyte gel can thus gradually lose the divalent cations ensuring the cross-linking bonds between the polymer chains, which results in a return of the gelled polyelectrolyte to its liquid form in solution and thus the loss of the mechanical strength of the gel .
- the present invention proposes to use a buffer to stabilize the mechanical properties of gelled polyelectrolyte capsules.
- the subject of the present invention is a composition
- a composition comprising: an aqueous composition (A) comprising a buffer having a pKa of from 4.0 to 8.0 and having at most one carboxylic acid function, and at least one capsule comprising a core, and a gelled envelope comprising a gelled polyelectrolyte chelated by divalent cations, said envelope completely encapsulating said core at its periphery, said capsule being devoid of eukaryotic cells.
- the composition of the invention typically corresponds to a mixture of the aqueous composition (A) and at least one capsule as defined above.
- mixing it is meant that the capsule (s) are fully immersed (i.e. immersed) in the aqueous composition (A) and that the gelled envelope of the capsules is in contact with the aqueous composition (A).
- the composition of the invention may comprise one or more additives or one or more active agents usually used in the cosmetics field.
- composition of the invention capsules typically corresponds to a suspension of at least one capsule as defined above in the aqueous composition (A).
- the use of such a buffer makes it possible to stabilize the mechanical properties of gelled polyelectrolyte capsules immersed in an aqueous composition comprising said buffer, and for a duration greater than one month and under conditions temperature ranging from 10 ° C to 50 ° C. More particularly, the use of said buffer makes it possible to maintain the polyelectrolyte gel in the gelled state and to avoid the migration of the divalent cations out of the network of polyelectrolyte chains.
- the stabilization of the mechanical properties of the capsules of the composition of the invention can be quantified by measuring the compressive strength (Rc) of capsules which have remained in an aqueous composition (A).
- the "compressive strength (Rc)” designates the maximum mass allowed by a capsule subjected to a crushing load and whose rupture is effected by bursting.
- the compressive strength is here expressed in grams and corresponds to the mass beyond which the capsule no longer supports the crushing load and therefore bursts.
- a reproducible method of measuring the compressive strength of capsules according to the invention is described in the examples below.
- a minimum compressive strength of 20 g is required for capsules of size greater than or equal to 2 mm to maintain acceptable properties. In the case of capsules of size approximately 5 mm, a minimum compressive strength of 50 g is preferable.
- the control of the pH of the aqueous composition (A) in which the gelled polyelectrolyte capsules are immersed makes it possible to obtain such a stabilizing effect.
- the buffers of the composition according to the invention do not chelate the divalent cations of the polyelectrolyte gel nor form a precipitate with said cations.
- the buffer is not capable of chelating Ca 2+ cations.
- buffer means a chemical species which, in aqueous solution, maintains the pH of the aqueous composition in which it is solubilized, despite the addition of small amounts of an acid or of a base, or despite a dilution.
- the buffer of the composition of the invention comprises at most one carboxylic acid function.
- the buffer of the composition of the invention can not be a dicarboxylic acid (such as malic acid) or a triacid carboxylic acid (such as citric acid). These compounds are known to destabilize calcium alginate gels (Aslani et al., Journal of Microencapsulation 1996, 13 (5), 601-614 and Augst et al., Macromolecular Bioscience 2006, 6 (8), 623-633). According to one embodiment, the buffer of the composition of the invention has no carboxylic acid function.
- the buffer of the composition of the invention comprises one or two sulphonic acid functions, preferably only one.
- the pKa of the buffer of the composition according to the invention is between 4.0 and 8.0.
- the pKa is from 5.0 to 8.0, preferably from 6.0 to 8.0.
- a buffer suitable for the implementation of the invention a buffer selected from the group consisting of HEPES, Bis Tris, MES, phosphate buffers, and mixtures thereof can be used.
- HEPES means 4- (2-hydroxyethyl) -1-piperazine ethane sulfonic acid (CAS No.
- HEPES has a pKa of 7.5 and is used to buffer an aqueous composition in a pH range of 6.8 to 8.2.
- Bis Tris refers to 2,2-bis (hydroxymethyl) -2,2 ', 2 "-nitrilotriethanol (CAS RN 6976-37-0) Bis Tris has a pKa of 6.5 and is used to buffer an aqueous composition in a pH range of 5.8 to 7.2.
- MES means 2- (N-morpholino) ethanesulfonic acid (CAS No. 4432-31 -9).
- MES has a pKa of 6.1 and is used to buffer an aqueous composition in a pH range of 5.5 to 6.7.
- phosphate buffer a buffer comprising dihydrogen phosphate and hydrogen phosphate ions.
- a phosphate buffer according to the invention can be prepared by dissolving monosodium or monopotassium phosphate and disodium or dipotassium phosphate in water.
- PBS phosphate buffered saline
- phosphate buffered saline phosphate buffered saline
- disodium phosphate (10 mM) monopotassium phosphate (1.76 mM)
- chloride of sodium 137 mM
- potassium chloride 2.7 mM
- PBS has a pKa of 7.2 and is used to buffer an aqueous composition in a pH range of 6.5 to 7.9.
- phosphate buffer By way of phosphate buffer, mention may also be made of the buffer prepared by dissolving disodium phosphate (0.44% by weight) and monopotassium phosphate (2.74% by mass) in water. Such a buffer has a pKa of 5.8.
- HEPES or PBS is used as a buffer.
- the buffer of the composition of the invention is present in a concentration of from 10 mM to 300 mM in the aqueous composition (A).
- the buffer is present in a concentration greater than 300 mM, and can for example go up to 1000 mM, or even up to 1500 mM.
- the buffer concentration is less than 250 mM, advantageously less than 200 mM, preferably less than 100 mM.
- the buffer can be used in a concentration of from 20 mM to 150 mM, preferably from 20 mM to 100 mM.
- the buffer is HEPES, it is preferably present in a concentration of from 10 mM to 1000 mM in the aqueous composition (A).
- the buffer is PBS, it is preferably present in a concentration of from 10 mM to 150 mM in the aqueous composition (A).
- the buffer is Bis Tris, it is preferably present at a concentration of from 10 mM to 300 mM in the aqueous composition (A).
- the buffer is MES, it is preferably present in a concentration of from 10 mM to 300 mM in the aqueous composition (A).
- composition of the invention may comprise a single capsule or a plurality of identical or different capsules.
- the gelled capsules of the composition of the invention also called “gelled polyelectrolyte capsules"
- the heart of the capsules is directly in contact with the gelled envelope, that is to say that there is no intermediate membrane between said core and said envelope.
- the capsules of the invention are necessarily devoid of eukaryotic cells, either in their heart, in their gelled envelope, or on the outer surface of said envelope.
- the gelled polyelectrolyte capsules are gelled alginate capsules, i.e. the polyelectrolyte is an alginate.
- the gelled polyelectrolyte capsules are gelled alginate capsules and the pKa of the buffer of the composition according to the invention is from 6.0 to 8.0.
- the heart of the capsules preferably comprises at least one active agent.
- the liquid heart may comprise a single active agent or a mixture of several active agents.
- active agent means a compound having a physiological effect beneficial on the element on which it acts. It aims for example to protect, maintain in good condition, cure, heal, perfume, flavor or color.
- the active agent is advantageously a cosmetic, dermo-pharmaceutical, pharmaceutical, perfume or food agent.
- the core may contain the active agent in the form of a pure liquid, or a solution of the active agent in a liquid solvent, or a dispersion such as an emulsion or suspension of the active agent in a liquid.
- the active agent when it is a cosmetic agent, it may be chosen from sodium hyaluronate or other moisturizing / repairing molecules, vitamins, enzymes, anti-wrinkle, anti-aging, protective / antiradical agents, antioxidants, soothing, softening, anti-irritant, tensing / smoothing, emollient, slimming, anti-cellulite, firming, shaping, draining, anti-inflammatory, depigmenting, whitening, self-tanning, exfoliating, stimulating cell renewal or stimulating cutaneous microcirculation, absorbing or filtering UV, anti-dandruff.
- sodium hyaluronate or other moisturizing / repairing molecules vitamins, enzymes, anti-wrinkle, anti-aging, protective / antiradical agents, antioxidants, soothing, softening, anti-irritant, tensing / smoothing, emollient, slimming, anti-cellulite, firming, shaping, draining, anti-inflammatory, depigmenting, whitening,
- a cosmetic agent that may be contained in the heart is for example cited in Council Directive 93/35 / EEC dated June 14, 1993.
- This product is for example a cream, an emulsion, a lotion, a gel and an oil for skin (hands, face, feet, etc.), a foundation (liquid, paste) a preparation for baths and showers (salts, mousses, oils, gels, etc.), a hair care product (hair dyes and bleaches ), a cleaning product (lotions, powders, shampoos), a hair care product (lotions, creams, oils), a styling product (lotions, lacquers, glossines), a product for shaving (soaps, mousses, lotions, etc.), a product intended to be applied to the lips, a sun product, a sunless tanning product, a product for whitening the skin, an anti-wrinkle product.
- the dermopharmaceutical agents more particularly designate agents acting on the skin.
- the active agent is a pharmaceutical agent
- it is advantageously chosen from anticoagulants, antithrombogenic agents, anti-mitotic agents, anti-proliferation agents, anti-adhesion agents, anti-migration agents, cell adhesion promoters, growth, antiparasitic molecules, anti-inflammatory drugs, angiogenics, angiogenesis inhibitors, vitamins, hormones, proteins, antifungals, antimicrobial molecules, antiseptics or antibiotics.
- the active agent when it is a perfuming agent, it may be in the form of a mixture.
- perfuming agents any type of perfume or fragrance, these terms being used here indifferently.
- perfumes or fragrances are well known to those skilled in the art and include, in particular, those mentioned, for example, in S. Arctander, Perfume and Flavor Chemicals (Montclair, NJ, 1969), S. Arctander, Perfume and Flavor Materials of Natural Origin. (Elizabeth, NJ, 1960) and in "Flavor and Fragrance Materials," 1991 (Allured Publishing Co. Wheaton, III, USA).
- the perfumes used in the context of the present invention may comprise natural products such as extracts, essential oils, absolutes, resinoids, resins, concretes, etc., as well as basic synthetic substances such as hydrocarbons, alcohols, aldehydes, ketones, ethers, acids, esters, acetals, ketals, nitriles, etc., including saturated and unsaturated compounds, aliphatic, alicyclic and heterocyclic compounds.
- the food agents are advantageously purees of vegetables or fruits such as mango puree, pear puree, coconut puree, cream of onions, leeks, carrots, or other preparations that may mix several fruits or vegetables.
- these are oils such as a food oil, such as olive oil, soybean oil, grape seed oil, sunflower oil, or any other oil extracted from the plants, as well as active ingredients.
- probiotics, yeasts, vitamins, minerals or oleoactives are examples of vegetables or fruits such as mango puree, pear puree, coconut puree, cream of onions, leeks, carrots, or other preparations that may mix several fruits or vegetables.
- oils such as a food oil, such as olive oil, soybean oil, grape seed oil, sunflower oil, or any other oil extracted from the plants, as well as active ingredients.
- probiotics, yeasts, vitamins, minerals or oleoactives such as probiotics, yeasts, vitamins, minerals or oleoactives.
- the heart may also include a coloring agent.
- the heart is liquid.
- the heart is gelled.
- the core When the core is gelled, it may contain a polyelectrolyte gel identical to the polyelectrolyte gel of the envelope.
- the heart when it is gelled, it may contain an aqueous solution of a gelling agent different from the polyelectrolyte of the envelope.
- the gelling agent is preferably selected from the group consisting of polysaccharides, galactomannans, polysaccharides, glycosaminoglycans and polyols.
- it is chosen from the group consisting of xanthan gum, carrageenan, carob, guar gum, gellan, hyaluronic acid, glycerol, propanediol, cellulose or its derivatives.
- a gelling agent When a gelling agent is present in the heart, it is typically present in a concentration of from 0.01% to 1% by weight relative to the total mass of the heart.
- the gelled envelope of the capsules also called “external envelope” is a gelled membrane comprising a polyelectrolyte in the gelled state chelated by divalent cations which ensures the mechanical strength of the capsules.
- the gelled envelope may also be referred to as "membrane” or "bark”.
- the gelled envelope has a thickness of less than 500 ⁇ , advantageously greater than 10 ⁇ , typically ranging from 25 ⁇ to 100 ⁇ .
- the gelled envelope is generally formed by a monolayer of a homogeneous material.
- the gelled envelope consists of a hydrogel comprising water and a polyelectrolyte chelated by divalent cations, and optionally a surfactant as described below.
- the polyelectrolyte present in the capsule shell is a divalent cation reactive polyelectrolyte.
- divalent cation reactive polyelectrolyte means a polyelectrolyte capable of passing from a liquid state in an aqueous solution to a gelled state under the effect of contact with a gelling solution containing divalent cations.
- divalent cations is meant in particular the cations of the alkaline earth metals selected for example from the calcium (Ca 2+ ), barium (Ba 2+ ) and magnesium (Mg 2+ ) cations.
- the divalent cations are calcium (Ca 2+ ) cations.
- the polyelectrolyte may in particular be a natural polysaccharide reactive with multivalent ions such as an alkaline alginate, a gellan, a pectin or a carrageenan.
- the polyelectrolyte is an alginate.
- Alginates are produced from brown algae called “laminar”, referred to as “sea weed”. Such alginates advantageously have a mass content of ⁇ -L-guluronate greater than about 50%, preferably greater than 55%, or even greater than 60%.
- the polyelectrolyte in the gelled state in the capsule shell is calcium alginate.
- the individual polyelectrolyte chains in the liquid state advantageously have a molar mass greater than 65,000 g / mol.
- the individual polyelectrolyte chains form, with the divalent cations, a coherent three-dimensional network that holds the liquid core and prevents its flow.
- the individual chains are held together and can not flow freely relative to each other. In this state, the viscosity of the formed gel is infinite.
- the three-dimensional polyelectrolyte gel contained in the envelope traps water (and a surfactant when present).
- the mass content of polyelectrolyte in the envelope is, for example, from 0.5% to 5% relative to the total mass of the envelope.
- the gelled envelope may further contain a surfactant.
- the surfactant is preferably an anionic surfactant, a nonionic surfactant, a cationic surfactant, or a mixture thereof.
- the molecular weight of the surfactant is between 150 g / mol and 10,000 g / mol, advantageously between 250 g / mol and 1500 g / mol.
- the surfactant is an anionic surfactant
- it is, for example, chosen from alkyl sulphates, alkyl sulphonates, alkyl aryl sulphonates, alkaline alkyl phosphates, dialkyl sulphosuccinates and alkaline earth salts of saturated or unsaturated fatty acids.
- These surfactants advantageously have at least one hydrophobic hydrocarbon chain having a number of carbons greater than 5 or even 10 and at least one hydrophilic anionic group, such as a sulfate, a sulfonate or a carboxylate linked to one end of the hydrophobic chain.
- the surfactant is a cationic surfactant
- it is for example chosen from alkylpyridium or alkylammonium halide salts such as n-ethyldodecylammonium chloride or bromide, cetylammonium chloride or bromide (CTAB) .
- CTLAB cetylammonium chloride or bromide
- These surfactants advantageously have at least one hydrophobic hydrocarbon chain having a number of carbon atoms greater than 5 or even 10 and at least one hydrophilic cationic group, such as a quaternary ammonium cation.
- the surfactant is a nonionic surfactant
- it is for example chosen from polyoxyethylenated and / or polyoxypropylenated derivatives of fatty alcohols, fatty acids, or alkylphenols, arylphenols, or from alkylglucosides, polysorbates and cocamides .
- the surfactant is sodium lauryl sulphate (SLS or SDS).
- SLS sodium lauryl sulphate
- the mass content of surfactant in the shell is greater than 0.001% and is advantageously less than 0.1%.
- the capsules have a substantially spherical shape and an outside diameter greater than 0.5 mm, advantageously less than 10 mm and preferably between 1 and 5 mm. They may also be referred to as "pearls”.
- the gelled envelope of the complex capsules is such that the volume ratio R v of the volume of the core to the volume of the gelled envelope is greater than 2, and is in particular greater than 5.
- This ratio R v is advantageously less than 50. It is for example between 5 and 10.
- the heart of the capsules contains a proportion of the polyelectrolyte present in the gelled envelope, in a concentration that is, however, less than the concentration of said polyelectrolyte in the gelled envelope.
- the ratio between the concentration of the polyelectrolyte in the core and the concentration of the polyelectrolyte in the gelled envelope is less than or equal to 0.1, preferably less than or equal to 0.05.
- the heart of the capsules is free of the polyelectrolyte present in the gelled envelope.
- the capsule is a so-called “simple” capsule, meaning that the core consists of a single internal phase, which may be aqueous or oily, said internal phase being placed directly in contact with the gelled envelope.
- a simple capsule is for example a capsule as described in the international application WO 2010/063937 in the name of the Applicant.
- a single capsule therefore comprises two distinct phases, an internal phase, preferably a liquid phase, and an external phase in the gelled state surrounding the internal phase.
- the active agent when present, may be contained in the inner phase or the outer phase. Preferably, the active agent is contained in the inner phase.
- the heart of a single capsule consists of a single internal phase, which can be aqueous or oily.
- aqueous phase means a phase having the property of solubilizing polar and hydrophilic compounds.
- An aqueous phase preferably comprises water and at least one active agent as described above, which is otherwise hydrophilic.
- ily phase means a phase having the property of solubilizing apolar compounds, such as fats, oils, lipids.
- An oily phase preferably comprises a fatty substance, an oil or a mixture of oils of plant, animal or mineral origin.
- a vegetable oil mention may for example be made of sweet almond oil, jojoba oil, palm oil, argan oil or phytosqualane.
- fatty substances examples include esters of fatty alcohols and / or fatty acids, such as isopropyl myristate, glycerol myristate, isononyl isononanoate and acid triglycerides. caprylic or capric acid, isopropyl palmitate and ethyl palmitate.
- mineral oil mention may be made, for example, of hydrogenated polyisobutylene, isododecane, paraffin oils or silicone oils.
- the capsule is a so-called “complex" capsule, meaning that the core comprises a single intermediate drop of an intermediate phase, the intermediate phase being placed directly in contact with the gelled envelope, and at least one internal drop of an internal phase disposed in the intermediate drop.
- a complex capsule is for example a capsule as described in the international application WO 2012/089820 in the name of the Applicant.
- the heart of a complex capsule can thus comprise a continuous intermediate phase within which there is only one drop of internal phase.
- the core comprises a continuous intermediate phase within which a plurality of internal phase drops (s) are located.
- the active agent of the heart when present, may be contained in the intermediate phase and / or in the internal phase of the heart of the complex capsule.
- the core of a complex capsule comprises an intermediate drop formed based on an aqueous intermediate phase and at least one or even a single macroscopic internal drop disposed in the intermediate drop and formed of an oily internal phase immiscible with the aqueous intermediate phase.
- the core of a complex capsule comprises an intermediate drop formed based on an oily intermediate phase and at least one, or even a single, macroscopic internal drop disposed in the intermediate drop and formed of an immiscible aqueous internal phase with the oily intermediate phase.
- aqueous phase and “oily phase” are as defined above.
- the intermediate drop of the heart is advantageously liquid.
- the intermediate drop is made based on a thixotropic intermediate phase, which is in the liquid state and destructured when it flows, but which is substantially solid or gelled at rest.
- liquid when it flows it is meant that the behavior of the intermediate phase is viscous, ie the deformation of the material depends not only on the stress applied but also on the duration during which this stress is applied. .
- One way to characterize this behavior is by a creep test using a rheometer on the sample, we apply a characteristic stress of the flows involved during the manufacturing and we trace the strain curve as a function of time ( data obtained with the rheometer software). If the curve has a non-zero slope at long times (more than 30 seconds), the intermediate phase can be considered as being liquid. If this slope is zero, the intermediate phase can be considered as solid.
- solid or gelled at rest it is meant that the behavior of the solid intermediate phase or gelled at rest, ie the deformation of the material depends only on the applied stress.
- One way to characterize this behavior is by a creep test using a rheometer, on the sample, a stress is applied characteristic of those undergone by the capsule at rest as a function of time (data obtained with the software of the rheometer). If the curve has a zero slope at long times (more than 30 seconds), the intermediate phase can be considered as solid. If this slope is non-zero, the intermediate phase can be considered as being liquid.
- the intermediate drop is gelled.
- the intermediate drop is for example formed by the gelling of a gelling product obtained by a temperature change, in particular by a temperature decrease of at least 10 ° C.
- gelation is obtained in the presence of ions, other molecules or certain conditions of pH or ionic strength.
- the intermediate drop may comprise one or more cosmetic, dermo-pharmaceutical, pharmaceutical, perfume or food active agents, as defined above.
- the intermediate drop may also include excipients, such as thickeners, or rheology modifiers.
- thickeners are, for example, polymers, cross-polymers, microgels, gums or proteins, including polysaccharides, celluloses, polysaccharides, silicone polymers and co-polymers, colloidal particles (silica, clays). , latex ).
- the intermediate drop may comprise solid particles, and in particular nacre particles.
- the intermediate drop is fully interposed between the inner drop and the gelled envelope.
- the entire inner surface of the gelled envelope is in contact with the intermediate drop, so that the intermediate drop keeps the inner drop completely away from the gelled envelope.
- the internal drop (s) may comprise one or more cosmetic, dermo-pharmaceutical, pharmaceutical, perfume or food active agents, as defined above.
- the capsule advantageously comprises a single internal drop disposed in the intermediate drop.
- the internal drop (s) are usually macroscopic.
- the maximum transverse dimension of each internal drop is greater than 150 ⁇ , and is in particular greater than
- the minimum volume of at least one internal drop is thus greater than 0.5% of the volume of the heart.
- the sum of the volumes of the or each internal drop is thus comprised from 0.5% to 65% of the total volume of the heart, in particular from 1% to 55% of the volume of the heart.
- Each internal drop advantageously has a spherical shape.
- the shape of the inner drop is different from a spherical shape, for example elliptical or lenticular.
- the internal phase constituting the internal drops is substantially immiscible with the intermediate phase constituting the intermediate drops.
- the capsule is a capsule called "solid", that is to say that the core also comprises a polyelectrolyte in the gelled state chelated by divalent cations, said polyelectrolyte being identical to that present in the envelope.
- the composition of the core and the composition of the envelope are identical and constitute a single phase.
- Such capsules may be prepared by simply driping into a gelling solution comprising divalent cations a composition comprising a polyelectrolyte in solution.
- the aqueous composition (A) in which the capsules of the composition of the invention are dipped may be liquid or gelled.
- the aqueous composition (A) When gelled, the aqueous composition (A) is in the form of an "aqueous gel", i.e. it is a solution comprising water and a gelling agent.
- gelling agent means a compound capable of giving a composition the consistency of a gel.
- the gelling agent is preferably selected from the group consisting of polysaccharides, galactomannans, polysaccharides, glycosaminoglycans and polyols.
- xanthan gum carrageenan, carob, guar gum, gellan, hyaluronic acid, glycerol, propanediol, cellulose or its derivatives.
- the aqueous composition (A) has a viscosity of less than 50 Pa.s as measured at 25 ° C., preferably less than 20 Pa.s.
- the aqueous composition (A) has a viscosity of 2 Pa.s at 15 Pa.s as measured at 25 ° C.
- Such viscosity of the aqueous gel allows a good suspension of the capsules, especially over a period of at least one month, at a temperature of 40 ° C.
- the composition (A) does not suspend the capsules, that is to say that they sediment in the composition (A).
- the aqueous gel is transparent so that the consumer can visualize the capsule. Its texture is chosen according to the texture that is desired for the composition of the invention.
- the viscosity is measured by the following method, in particular described in the international application WO 2013/132082 in the name of the Applicant.
- a Brookfield type viscometer with a mobile (Spindle) of size (No.) 05 was used. About 150 g of solution were placed at 25 ° C. in a 250 ml beaker with a diameter of about 7 cm. so that the height of the volume occupied by the 150 g of solution is sufficient to reach the gauge marked on the mobile. Then, the viscometer is started at a speed of 10 rpm and the value displayed on the screen is expected to be stable.
- the weight percentage of water of the aqueous gel is at least 70%, especially 70% to 85%, preferably 70% to 80%, relative to the total mass of the composition (A) .
- the aqueous composition (A) may also comprise a cosmetic, dermopharmaceutical, pharmaceutical, fragrance or food agent as defined above.
- the aqueous composition (A) may also comprise a preservative, a coloring agent and / or a nacre.
- the mass ratio between the aqueous composition (A) and the capsules is from 30/70 to 70/30, preferably from 40/60 to 60/40.
- the present invention also relates to a process for preparing the composition according to the invention, comprising:
- the aqueous composition (A) can be prepared by mixing the various ingredients in the water and then adding the buffer.
- the present invention also relates to the use of a buffer having a pKa of from 4.0 to 8.0 and having at most one carboxylic acid function, to maintain above a minimum value equal to 20 g the compressive strength (Rc) of capsules as defined above, when immersed in an aqueous composition comprising said buffer.
- the pKa of the buffer is from 5.0 to 8.0, preferably from 6.0 to 8.0.
- the buffer may be one of the buffers described above.
- the compressive strength (Rc) is as defined above. It has been observed that, surprisingly, the use of such a buffer makes it possible to maintain the compressive strength (Rc) of gelled alginate capsules immersed in an aqueous composition comprising said buffer, and for a greater duration at one month and under temperature conditions ranging from 10 ° C to 50 ° C. The maintenance of the compressive strength (Rc) is explained by the stabilization of the alginate in the gelled state, in particular by the inhibition of the migration out of the network of alginate chains of the divalent cations chelating said alginate .
- the minimum value of Rc may be 40 g, or even 50 g.
- the minimum value of Rc may be 65 g.
- the composition of the invention is a cosmetic composition in association with a cosmetically acceptable vehicle.
- the present invention also relates to a non-therapeutic cosmetic treatment method of the skin comprising a step of applying to the skin at least one layer of the composition according to the invention.
- This process is preferably carried out with a composition comprising capsules whose active agent (s) are non-therapeutic cosmetic active agents.
- the invention also relates to the cosmetic use of the cosmetic composition described above.
- a cube of sodium alginate is prepared by dissolving sodium alginate (5 g) in
- the gelled cube obtained is then placed in pure water maintained around 25 ° C.
- the calcium alginate gel begins to weaken after one month at 50 ° C, and liquefies completely after 3 months at 50 ° C.
- Complex capsules as defined in the description were prepared according to the method described in WO 2012/089820. They have a diameter of about 4 mm.
- the inner drop consists of argan oil, the intermediate drop is an aqueous solution and the gelled casing is a calcium alginate hydrogel.
- the capsules have the following composition:
- the capsules thus prepared were immersed in pure water maintained at 50 ° C.
- the mechanical strength of the capsules was then measured over time by measuring the compressive strength, called Rc. This property corresponds to the ability of the capsules to resist compression.
- the principle is to exert a stress at a constant speed on a capsule and to measure what is the force required to rupture the capsule.
- the method described in the international application WO 2013/132083 was used.
- the capsule is deposited on a scale and a stress is exerted at a constant speed by means of a syringe piston filled by a constant flow of oil, by means of a syringe pump (60 ml / h) .
- a syringe pump 60 ml / h
- the compressive strength, Rc is given by the limit mass obtained before rupture of the capsule. It is analytically given when a mass decrease of more than 1% is observed on the scale.
- the Rc (in g) of a sample of capsules is determined by realizing the mean and standard deviation associated with Rc measurements of 10 capsules randomly selected from the lot.
- the results of the Rc of the capsules as a function of the immersion time in water are given in Table 1.
- Gelled calcium alginate capsules therefore have a mechanical resistance which degrades over time in pure water. There is a very rapid decrease of Rc in the first days.
- Example 3 Alginate gel capsules immersed in an aqueous gel pH adjusted initially
- Example 2 was reproduced by replacing the osmosis water with an aqueous gel whose pH is initially adjusted by adding acid / base (pH adjusted to 6, 8 or 10).
- the aqueous gel has the following composition: Trade Name INCI Name supplier% gel (m / m)
- the alginate gel of the capsules loses its mechanical strength in less than one month (at room temperature or at 50 ° C.), regardless of the pH adjusted initially.
- Example 3 Gelled alginate capsules immersed in a buffered aqueous gel
- Example 2 was reproduced by replacing the osmosis water with an aqueous gel comprising a buffer (corresponding to the aqueous composition (A) described above) in a concentration in buffer in the aqueous gel of 500 mM.
- a buffer corresponding to the aqueous composition (A) described above
- the aqueous gel has the following composition:
- the other PBS, HEPES, MES, ACES, PIPES and Bis Tris buffers did not lead to the deterioration of the alginate gel, and made it possible to maintain the alginate capsules withstand over time (for at least one month at 50 ° C).
- HEPES, MES and Bis Tris buffers maintain the mechanical strength of the capsules, even after 135 days.
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Abstract
Description
Claims
Priority Applications (3)
Application Number | Priority Date | Filing Date | Title |
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CN201480062910.0A CN105899182B (zh) | 2013-11-18 | 2014-11-14 | 包含由缓冲剂稳定的胶凝胶囊的组合物 |
EP14798885.1A EP3071169A1 (fr) | 2013-11-18 | 2014-11-14 | Composition comprenant des capsules gélifiées stabilisées par un tampon |
US15/035,822 US10596081B2 (en) | 2013-11-18 | 2014-11-14 | Composition comprising gelled capsules stabilized by a buffer |
Applications Claiming Priority (2)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
FR1361311A FR3013218B1 (fr) | 2013-11-18 | 2013-11-18 | Composition comprenant des capsules gelifiees stabilisees par un tampon |
FR1361311 | 2013-11-18 |
Publications (1)
Publication Number | Publication Date |
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WO2015071433A1 true WO2015071433A1 (fr) | 2015-05-21 |
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ID=50976679
Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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PCT/EP2014/074663 WO2015071433A1 (fr) | 2013-11-18 | 2014-11-14 | Composition comprenant des capsules gélifiées stabilisées par un tampon |
Country Status (5)
Country | Link |
---|---|
US (1) | US10596081B2 (fr) |
EP (1) | EP3071169A1 (fr) |
CN (1) | CN105899182B (fr) |
FR (1) | FR3013218B1 (fr) |
WO (1) | WO2015071433A1 (fr) |
Cited By (8)
Publication number | Priority date | Publication date | Assignee | Title |
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WO2018015197A1 (fr) | 2016-07-20 | 2018-01-25 | Capsum | Série de capsules et procédé de fabrication, composition cosmétique et traitement cosmétique |
WO2019002371A1 (fr) * | 2017-06-28 | 2019-01-03 | Nestlé Skin Health Sa | Gel de glycosaminoglycane avec tampon bis-tris |
FR3072575A1 (fr) * | 2017-10-23 | 2019-04-26 | Kevolis | Composition changeant de couleur et/ou de gout pour soins buccaux a base de capsules d’alginate |
FR3079149A1 (fr) * | 2018-03-26 | 2019-09-27 | Capsum | Serie de particules a coeur au moins en partie gelifie |
FR3089418A1 (fr) * | 2018-12-05 | 2020-06-12 | V. Mane Fils | Capsules à base d’amidon riche en amylose et leur procédé de fabrication |
WO2020092104A3 (fr) * | 2018-10-29 | 2020-07-30 | The Procter & Gamble Company | Composition liquide encapsulée |
DE102019201362A1 (de) * | 2019-02-04 | 2020-08-06 | Beiersdorf Ag | Partikeldispersion enthaltend Polymere |
DE102019201364A1 (de) * | 2019-02-04 | 2020-08-06 | Beiersdorf Ag | Kosmetisches Produkt enthaltend Kapseln |
Families Citing this family (2)
Publication number | Priority date | Publication date | Assignee | Title |
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ES2849750B2 (es) * | 2020-02-19 | 2022-07-29 | Fingerclik S L | Capsula galenica rompible |
WO2021242838A1 (fr) * | 2020-05-26 | 2021-12-02 | One Fun Company, Inc. | Compositions comprenant des produits de soins personnels et procédés associés |
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FR2986165A1 (fr) * | 2012-01-31 | 2013-08-02 | Capsum | Procede de preparation de capsules rigidifiees |
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- 2014-11-14 EP EP14798885.1A patent/EP3071169A1/fr not_active Withdrawn
- 2014-11-14 US US15/035,822 patent/US10596081B2/en active Active
- 2014-11-14 CN CN201480062910.0A patent/CN105899182B/zh active Active
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Cited By (11)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
WO2018015197A1 (fr) | 2016-07-20 | 2018-01-25 | Capsum | Série de capsules et procédé de fabrication, composition cosmétique et traitement cosmétique |
US10940098B2 (en) | 2016-07-20 | 2021-03-09 | Capsum | Series of capsules and method of manufacture, cosmetic composition and cosmetic treatment |
WO2019002371A1 (fr) * | 2017-06-28 | 2019-01-03 | Nestlé Skin Health Sa | Gel de glycosaminoglycane avec tampon bis-tris |
FR3072575A1 (fr) * | 2017-10-23 | 2019-04-26 | Kevolis | Composition changeant de couleur et/ou de gout pour soins buccaux a base de capsules d’alginate |
WO2019081325A1 (fr) * | 2017-10-23 | 2019-05-02 | Kevolis | Composition changeant de couleur et/ou de goût pour soins buccaux à base de capsules d'alginate |
FR3079149A1 (fr) * | 2018-03-26 | 2019-09-27 | Capsum | Serie de particules a coeur au moins en partie gelifie |
WO2020092104A3 (fr) * | 2018-10-29 | 2020-07-30 | The Procter & Gamble Company | Composition liquide encapsulée |
FR3089418A1 (fr) * | 2018-12-05 | 2020-06-12 | V. Mane Fils | Capsules à base d’amidon riche en amylose et leur procédé de fabrication |
WO2020115138A3 (fr) * | 2018-12-05 | 2020-08-06 | V. Mane Fils | Capsules à base d'amidon à haute teneur en amylose et leur procédé de fabrication |
DE102019201362A1 (de) * | 2019-02-04 | 2020-08-06 | Beiersdorf Ag | Partikeldispersion enthaltend Polymere |
DE102019201364A1 (de) * | 2019-02-04 | 2020-08-06 | Beiersdorf Ag | Kosmetisches Produkt enthaltend Kapseln |
Also Published As
Publication number | Publication date |
---|---|
FR3013218A1 (fr) | 2015-05-22 |
EP3071169A1 (fr) | 2016-09-28 |
CN105899182B (zh) | 2020-06-26 |
FR3013218B1 (fr) | 2016-07-29 |
CN105899182A (zh) | 2016-08-24 |
US20160296432A1 (en) | 2016-10-13 |
US10596081B2 (en) | 2020-03-24 |
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