FR2906135A1 - Preparing an active ingredient useful for immediate tightening effect of skin, comprises extracting and purifying high molecular weight polysaccharides from oat bran and/or fibers, solubilizing and stabilizing the polysaccharides in water - Google Patents

Abstract

Preparation of an active ingredient for immediate tightening effect of skin, comprises extracting and purifying polysaccharides of high molecular weight from oat bran and/or fibers, solubilizing and stabilizing the polysaccharides in water. Independent claims are included for: (1) an active ingredient obtained by implementing the process characterized by the rate of solid matter comprised between 20-200 g/l, a pH of 4-8, a total sugar content of 19-190 g/l and presence of polysaccharides of high molecular weight, having a degree of polymerization greater than 40; and (2) a composition comprising the active ingredient in a limpid gel, opaque gel, emulsified gel or non-ionic, anionic or cationic emulsion.

Description

METHOD FOR OBTAINING AN ACTIVE INGREDIENT WITH IMMEDIATE TENSE EFFECT OF THE

  The present invention relates to a process for obtaining an active ingredient rich in high molecular weight polysaccharides derived from fibers and / or oat bran, having an immediate tightening effect on the skin. The invention also relates to the active ingredient that can be obtained by this process, its uses and the associated cosmetic compositions. To look younger, many people want to firm their skin and mitigate unsightly physical changes directly visible skin aging. The aging of the skin results from various alterations caused by both genetic and environmental factors. It is manifested in particular by the loss of the mechanical strength and the viscoelastic and lifting properties of the dermis. The skin then tends to expand under the influence of its own weight, thus causing surface deformations, the formation of wrinkles and unsightly folds. The epidermis also loses its thickness and the cutaneous microrelief is modified. To fight against this phenomenon, we are therefore looking for cosmetic active ingredients that make it possible to both lift, smooth the cutaneous microrelief, and improve the viscoelastic properties of the skin. Until now, to meet their lifting needs, formulators had at their disposal two types of substances: synthetic polymers, sticky, often difficult to formulate because only soluble in alcohol, and soluble proteins; in water, but may be responsible for skin reactions of allergic type. Also, the present invention aims at overcoming the drawbacks of the prior art by proposing a process for obtaining an active ingredient with immediate, effective, soluble and stable tensor effect in water, of vegetable origin and limiting to maximum protein content. For this purpose, the subject of the invention is a process for obtaining an active ingredient with an immediate tensor effect, characterized in that it consists in extracting and purifying high molecular weight polysaccharides from bran and / or oat fiber, to solubilize and stabilize these polysaccharides in water. The active ingredient according to the invention can be obtained from simple oat fiber and / or from oat bran, a residue of oatmeal obtained from the pericarp of grains which, in addition to the fibers, contains proteins, mineral salts and vitamins.

Advantageously, the active ingredient obtained, rich in high molecular weight polysaccharides, provides a tight and tonic skin feeling and has an immediate tightening effect characterized by smoothing the skin microrelief and improving the mechanical properties of the skin. The present invention is now described in detail based on nonlimiting examples of compositions, as well as on test results grouped into tables. The method according to the present invention comprises at least two essential steps: a step of solubilizing its and / or oat fibers in a basic solution; and a step of successive or simultaneous enzymatic hydrolysis (s) of the polysaccharides contained in the bran and / or oat fibers, so as to facilitate their solubilization without breaking their molecular structure. According to one embodiment of the invention, to facilitate the solubilization of the polysaccharides, at least one solubilizing adjuvant is added to the basic solution, preferably a salt, a polyphosphate and / or an oxidant. The alkaline concentration of the basic solubilization solution can be adjusted so that the physical properties of the polysaccharides are not altered upon hydrolysis to simple sugars.

Preferably, the method according to the present invention also comprises a deproteinization step. According to a preferred embodiment, the process according to the invention comprises the following succession of steps: solubilization of a bran and / or oat fiber at a rate of 30 g / l to 300 g / l, more particularly 50 g / l at 150 g / l, in a basic solution containing a solubilization adjuvant, - successive or simultaneous enzymatic hydrolysis (s) of the polysaccharides, - inactivation by thermal or chemical treatment, to block the enzymatic reactions, separation of the soluble and insoluble phases by filtration, decantation and / or centrifugation, successive concentrations, deproteinization by precipitation or selective adsorption, purification of the active fraction containing the high molecular weight polysaccharides by ultrafiltration, and sterile filtration. .

Advantageously, the method according to the invention allows the preservation of native polysaccharides derived from bran and / or oat fibers, while facilitating the industrial feasibility of the active ingredient.

II / CHARACTERIZATION OF THE ACTIVE PRINCIPLE OBTAINED ACCORDING TO THE INVENTION FROM ITS OIL AND / OR OIL FIBERS II.1 / Dry matter The dry matter content is measured by oven drying at 105 ° C of a sample initial weight given until a constant weight is obtained.

The solids content is between 20 and 200 g / l, more particularly between 60 and 110 g / l. II.2 / pH measurement The pH measured by the potentiometric method at ambient temperature leads to values between 4 and 8, more particularly between 15 and 6. II.3 / Determination of total sugar content The DUBOIS method (DUBOIS M. et al. [1956], Analytical Chemistry, 28, No. 3, pp. 350-356) is used. In the presence of concentrated sulfuric acid and phenol, the reducing sugars give a yellow-orange compound. From a standard range, the total sugar content of a sample can be determined. The total sugar content of the active ingredient according to the present invention is from 19 to 190 g / l, preferably from 57 to 105 g / l.

The ratio of total sugars to solids content for the active ingredient according to the present invention is greater than 50%, preferably 80%.

II.4 / Average degree of polymerization of the polysaccharides The average degree of polymerization of the polysaccharides is determined by the ratio of the level of total sugars, on the ratio of reducing sugars. The dosage of reducing sugars is carried out as follows: the active ingredient is assayed in the presence of a solution of 4-hydroxybenzoic hydrazide in 0.5M hydrogen chloride and a 0.5M sodium hydroxide solution, a standard range is made with glucose, and the absorbance at 410 nm is measured to determine the reducing sugar content of the active ingredient relative to the glucose range. The average degree of polymerization of the polysaccharides of the active principle according to the present invention is greater than 40, preferably greater than 60.

II.5 / Size of polysaccharides The size distribution of the polysaccharides obtained by carrying out the process according to the invention is carried out by studying the chromatograms. The polysaccharides obtained by carrying out the process according to the invention are polysaccharides of high molecular weight. They have a polysaccharide size between 30 and 2000 kDa. Preferably 50% of the polysaccharide fraction has a size of between 70 and 700 kDa.

III / EVALUATION OF THE EFFECT OF THE ACTIVE INGREDIENT OBTAINED ACCORDING TO THE INVENTION FROM OIL SOUND III-1 / Evaluation of the tensor effect by Cutometer This study aims to evaluate the tensor effect of active ingredient obtained according to the invention from oat bran. The study is performed on volunteers using a cutometer. A Cutometer is a device with a probe that is applied to the skin in which a constant depression is maintained. The depth of penetration of the skin under the effect of aspiration is measured.

The skin, subjected to these depressions, tires more or less quickly and the response times as well as the measured amplitudes make it possible to determine parameters, in particular: an elastic component, Ue, which corresponds to an instantaneous deformation, and Uf, which corresponds to extensibility. If Ue decreases, the skin is less flexible, so more tense. If Uf decreases, the skin is less stretchy, so more tense as well. The operating protocol is as follows: a zone is determined on the forearms of the volunteers, and a first series of measurements is carried out with the cutometer; the active ingredient derived from the oat bran obtained according to the invention is applied; at 4% in emulsion or placebo on the determined zone, and - two hours after the application, a new series of measurements is carried out on the determined zone.

The reference results used are BSA (bovine serum serum) assayed at 4%. The results obtained for the active principle derived from oat bran according to the invention are expressed relative to placebo in the following table: Cosmetic efficacy / placebo (AUf) (Mie) -5.0% -7.1% -8.4% -9.9% BSA 4% Active ingredient according to the invention derived from oat bran It is found that the active ingredient according to the invention reduces the elastic component and the extensibility of the skin: it presents a immediate tightening effect of the skin. III-2 / Evaluation of the tensor effect in sensory analysis The objective of this study is to quantify in vivo the tensor effectiveness of the active principle according to the invention obtained from oat bran formulated at 10% in gel against placebo.

The sensory evaluation test consists in having the tightening and non-sticking sensation blindly evaluated by a panel of experts. The study is carried out on 15 healthy volunteers at the level of the eye and crow's feet. The operating protocol is as follows: at T minus 5 minutes, the volunteers remove the selected eye and crow's feet; at T0 8Op1 of a gel to be tested is applied: placebo gel, gel containing 10% of the active ingredient according to the invention obtained from oat bran, gel containing 5% BSA, gel containing 10% BSA and gel containing 20% BSA, and - at T 3 minutes, T 5 minutes and T 10 minutes, the tensor sensation is evaluated on a scale of 0 to 10, using a slider. The analysis of the scales is carried out by the sum of the scores at three times.

2906135 8 The different gels are randomly tested over several days (one gel per day). The results obtained are shown in the table below Sum of the scores of the 3 times Placebo 4.1 Active ingredient according to the invention derived from 13.6 oat bran 10% SAB 5% 8.2 SAB 10% 12, 9 SAB 20% 14.6 5 It is noted that after a single application, the experts recognize the active principle derived from oat bran as a tensor, non-sticky, and the score has an efficiency of 13.6, higher than that of SAB dosed at 10%. IV / COSMETIC COMPOSITION INCLUDING THE ACTIVE INGREDIENT ACCORDING TO THE INVENTION: The present invention also covers the cosmetic compositions including the active ingredient according to the present invention in different galenical forms, in particular gel, solution, emulsion, cream, etc. It is then appropriate to to analyze the stability of the dosage forms including the active ingredient according to the invention, this in proportions of between 1 and 5%.

The stability is characterized by a lack of precipitation of the active, an absence of creaming and a lack of phase shift. Formulations which have shown a physical stability including 5% of active principle according to the invention. Clear gel: Carbopol: 0.5% with Triethanolamine: qsp 20 pl-I = 6.5 2906135 9 Phenonip: 0.7% - Active ingredient: 5.0% - Water: 93.8% Opaque gel: - Sepigel 305 : 2.0% 5 - Phenonip: 0.7% - Active ingredient: 5.0% - Water: 92.3% Emulsified gel: - Montanov 202: 3.0% - Isopropyl palmitate: 12.0% Phenonip: 0.7% - Viscolam AT 64: 2.0% - Active ingredient: 5.0% - Water: 77.3% Non-ionic emulsion: -Montanov 202: 3.0% - Simulsol 165: 2.0% - Isopropyl palmitate: 20.0% Phenonip 0.7% Active ingredient 5.0% Water 69.3% Anionic emulsion 20.0% - Phenonip: 0.7% Active ingredient 5.0% 25 - Water: 63, 8% Cationic emulsion: Quaternium-82: 5.0% - Cetyl alcohol: 2.0% - Cetearyl alcohol: 1% PEG100 stearate: 1% - Isopropyl palmitate: 15.0% - Phenonip: 0.7% - Active ingredient: 5.0% - Water: 70.3% In addition, tests have shown the compatibility of the principle active with the raw materials used in cosmetics.

Claims (12)

  1. Process for obtaining an active ingredient with an immediate tensing effect on the skin, characterized in that it consists in extracting and purifying high molecular weight polysaccharides from bran and / or oat fibers, solubilize and stabilize these polysaccharides in water.   2. Production process according to claim 1, characterized in that it comprises at least the two following stages: solubilization of bran and / or oat fibers in a basic solution, and enzymatic hydrolysis (s) ( s) successive or simultaneous polysaccharides contained in the sound and / or oat fibers.   3. Production process according to claim 2, characterized in that it comprises a deproteinization step.   4. Production process according to any one of the preceding claims, characterized in that it comprises the succession of the following steps: - solubilization of bran and / or oat fiber in a basic solution, at a rate of 30 g / I to 300 g / I, - enzymatic hydrolysis (s) successive (s) or simultaneous (s) of the polysaccharides contained in the bran and / or cereal fibers, - inactivation by heat treatment or chemical, to block the reactions enzymatic, -separation of soluble and insoluble phases by filtration, decantation, and / or centrifugation, - successive concentration (s), - deproteinization by precipitation or selective adsorption, - purification of the active fraction containing the high polysaccharides molecular weight by ultrafiltration, and sterilizing filtration.   5. Production process according to claim 4, characterized in that the solubilization of bran and / or cereal fibers in a basic solution is at a rate of 50 g / l to 150 g / l.   6. Production process according to one of claims 2 to 5, characterized in that at least one solubilizing adjuvant is added to the basic solution.   7. Production process according to claim 6, characterized in that the solubilization adjuvant is a salt, a polyphosphate and / or an oxidant.   8. Active ingredient obtained by the implementation of the method according to one of the preceding claims, characterized by the following parameters - solids content of between 20 and 200 g / l, - pH between 4 and 8, 15 - content in total sugars between 19 and 190 g / l, - presence of polysaccharides of high molecular weight, having a degree of polymerization greater than 40.   9. Active ingredient according to claim 8, characterized by the following parameters: dry matter content between 60 and 110 g / l, pH between 5 and 6, total sugar content of between 57 and 105 g. I - presence of high molecular weight polysaccharides having a degree of polymerization greater than 60.   10. Composition comprising the active ingredient according to one of claims 8 or 9, characterized in that it consists of a clear gel, an opaque gel, an emulsified gel, a nonionic emulsion, an anionic emulsion or a cationic emulsion. 2906135 13   11. Use of high molecular weight polysaccharides obtained from bran and / or oat fibers and by carrying out the method according to one of claims 1 to 7, for incorporation into a cosmetic composition intended to have an effect. immediate skin tensor. 5   12. Use of high molecular weight polysaccharides obtained from bran and / or oat fibers and by carrying out the method according to one of claims 1 to 7, for incorporation into a cosmetic composition intended to provide a skin. tense and tonic.