FR3063902A1 - PROCESS FOR THE PRODUCTION OF POWDERS FOR MAKE - UP OR COSMETIC SKIN CARE AND COSMETIC COMPOSITION COMPRISING THE SAME. - Google Patents

Abstract

The invention relates to a powder manufacturing process for makeup or cosmetic care of the skin. The invention also comprises a powder-based cosmetic composition obtained from said process as well as the use of this powder for the preparation of a cosmetic composition.

Description

063 902

70250 ® FRENCH REPUBLIC

NATIONAL INSTITUTE OF INDUSTRIAL PROPERTY © Publication number:

(only to be used for reproduction orders) © National registration number

COURBEVOIE © Int Cl ⁸ : A 61 K8 / 9789 (2017.01), A 61 K8 / 97, 8/19, A 61Q1 / 12, 1/00, 19/00

A1 PATENT APPLICATION

©) Date of filing: 15.03.17. © Applicant (s): CONSTANCE ADELINE - FR, LAM- (© Priority: BEFtT JULIE— FR and AKBAFI SULAIMAN — TR. @ Inventor (s): CONSTANCE ADELINE. (© Date of public availability of the request: 21.09.18 Bulletin 18/38. ©) List of documents cited in the report preliminary research: Refer to end of present booklet (© References to other national documents ® Holder (s): CONSTANCE ADELINE, LAMBERT related: JULIE, AKBAR SULAIMAN. ©) Extension request (s): © Agent (s): TOUROUDE & ASSOCIATES.

PROCESS FOR THE MANUFACTURE OF POWDERS FOR MAKEUP OR COSMETIC SKIN CARE AND COSMETIC COMPOSITION COMPRISING THE SAME.

The subject of the invention is a method for manufacturing powder intended for making up or cosmetic care of the skin. The invention also includes a cosmetic composition based on powder obtained from said process as well as the use of this powder for the preparation of a cosmetic composition.

FR 3 063 902 - A1

The subject of the invention is a process for manufacturing powder intended for make-up or cosmetic care of the skin. The invention also includes a cosmetic composition based on powder obtained from said process as well as the use of this powder for the preparation of a cosmetic composition.

Cosmetic make-up or cosmetic skin care consists mainly of pigments which can be combined with pearlescent agents, fillers and fatty substances and with water in sometimes complex form systems. They generally consist of oily and / or aqueous phases. The good dispersion of these pigments, fillers and / or nacres in one or the other of these phases is essential.

Inorganic pigments, especially of mineral or synthetic origin, can be used for their coloring or protective power in cosmetic products. The pigments are insoluble in water or oil and can be of mineral, organic or even vegetable origin. They serve to add color to the cosmetic product but also can be used to modify the skin color during the use and application of makeup product. In natural makeup products, it is the mineral pigments that are most often used.

These pigments are asked to be able to disperse homogeneously with the desired color rendering and while having good stability when they are formulated.

The fillers, in particular of mineral origin, are generally introduced into make-up products as bulking agents, compacting agents, touching agent, for their visual effect (soft focus, dullness, etc.) and / or as an anti-caking agent.

Pearlescent (or light reflectors), mineral or synthetic are used as pigments and will bring coloring and light effects.

Unfortunately, inorganic pigments, such as metal oxides or composite inorganic pigments (such as pearlescent pigments), as well as fillers, tend to aggregate naturally due to their size, high density and natural affinity, especially when attempts to disperse them in aqueous or non-toxic solvents.

In addition, these pigments, like the fillers, tend to aggregate also when they are stored in the form of powder before their formulation and their final use, which makes their storage and their conservation in raw form after their production difficult.

The good dispersion of pigments and fillers in fatty substances is a very important point, but not only. Other performance criteria are to be taken into consideration such as:

• Dispersion in oils • Hydrophobicity • Skin affinity • Pleasant sensation on application • Good spreading on the skin • Low surface activity, or • Sebum control

Surface treatment techniques have been developed to meet these expectations.

Generally, the surface of inorganic pigments such as untreated metal oxides or fillers contains numerous hydroxyl groups with which the water molecules can easily combine. However, by using these surface hydroxyl groups, these pigments or charges can be modified by physicochemical adsorption, hydrogen bonding or other reactions. When, for example, these pigments or fillers come into contact with a polymer solution, the polymer molecule will remain bound to the surface of the pigment.

Thus, the primary benefit of applying an organic compound to the surface of different minerals is that they will have comparable surface properties and therefore that they will disperse homogeneously in the fatty or aqueous liquid phase.

Organic compounds having functional groups such as phosphate, amine, amide, carboxylic or hydroxyl can therefore be attached to the surface of these pigments by chemical adsorption, hydrogen bonding or electrical charge.

There are mainly two methods of processing these pigments or fillers:

• One is called the dry process in which the processing agents are simply added to the pigment or to the filler in a blender.

• The other, the wet process, consists in dissolving the treatment agents in a solvent, which can be water, and then introducing this solution into a tank containing the pigment or the filler previously dispersed in a liquid phase. . The solvent or water is then removed. The pigment or the treated filler is then dried and finely ground. (The Cosmetics Observatory, 2016.)

The dry forms of pigment or filler particles are in the form of agglomerates. Under the conditions of the dry process, the treatment material will be applied to the surface of these agglomerates. After grinding, the untreated internal parts of these agglomerates will emerge and this will result in poor homogeneity of the treatment.

In the wet process, the entire system is in the liquid phase. The molecules of the treatment material more easily penetrate the agglomerates and can be fixed on almost the entire surface of the particles.

The wet treatment is more homogeneous and provides better stability to cosmetic formulations.

Eco-design is attracting more and more companies. In the cosmetic industry in particular, it makes it possible to offer superior quality products while integrating sustainable development at the heart of the product's life cycles (see http://arehives.leseehos.fr/arehives/cerele/2011/06 / 23 / cerele 35959.htm # phkc2cAh fBaioYxZ.99).

On the basis of these treatments, to design the treatment of pigments or fillers from a natural product, the “classic” method would be to extract, purify and first select from this natural product the different fractions functional organics, such as phosphate, amine, amide, carboxylic or hydroxyl (see column "Step 1" in Figure 1), before grafting these functions onto the surface of the pigments, fillers and / or nacres contained in the powders used for makeup cosmetics and skin care, this grafting step is necessarily followed by at least one filtration step (sieving) and drying in the best of cases by wet or dry selected (see column 2 ^nd "Step 2" in Figure 1).

This last dehydration-drying step, on the other hand, serves to recover a functionalized and activated powder which will have better conservation. Such a process represents many steps (at least 9 to 10, see Figure 1).

Thus, in an eco-design framework, it would be desirable to be able to have a simpler method of treating a powder intended for a cosmetic composition and containing a pigment, a filler and / or a mother-of-pearl, a method using uses a natural active ingredient capable of achieving maximum functionalization of the constituents of this powder without altering either the quality of the make-up powders or this active ingredient, this with good hydration performance for the skin.

This is precisely the object of the present invention.

The object of the present invention is to propose new cosmetic compositions based on powders, the properties of which are improved, in particular the moisturizing properties and better availability of the moisturizing active agents for the skin, while ensuring comfort and hold of the powder on the skin. .

The invention also aims to simplify current industrial processes by proposing a method for modifying the surface of the powders used in these cosmetic compositions which is simple and easy to implement compared with the existing methods of the prior art which make it possible to be used reproducible and on an industrial scale in the cosmetic field.

The inventors have demonstrated that bringing a powder comprising or consisting of pigments and / or filler into contact with a crude vegetable extract, and in particular fruit, after grinding in the aqueous phase and in a hydrolysing medium makes it possible to modify as desired the surface of these pigments and / or fillers, this thanks to the active agents simultaneously released by this plant extract, in particular film-forming agents such as polysaccharides, humectants such as polyols and osmolytes such as simple sugars or galacturonic acid.

The inventors have demonstrated that the presence of these three types of agents would make it possible to obtain final powders for cosmetic use having the desired properties as improved hydrating power and better availability and persistence of hydration, compared to using a purified active ingredient.

The inventors have been able to demonstrate that it is possible to directly use a crude plant extract comprising such functions for the treatment of these powders without the need to extract and purify the functional compounds from these crude plant extracts. .

In addition, and in an interesting and surprising manner, the use of such crude extracts also makes it possible to reduce the process for treating these powders to 4 essential steps (see Figure 2).

In addition, the inventors have demonstrated that the powders thus treated have very interesting moisturizing properties with in particular better hydration and / or better availability of moisturizing active agents for the skin than that which could be obtained with a process using using a purified active ingredient.

The inventors have demonstrated, for example, these surprising properties of these powders obtained from a mixture of raw ground chestnut and pigments of the metal oxide type.

It is therefore an object of the present invention to be able to provide a simple and easy method for implementing surface modification of a powder intended for a cosmetic composition and containing a pigment and / or a filler and / or if necessary a mother-of-pearl.

The inventors have demonstrated that such a modification of the surface of said substrate (pigment, filler or mother-of-pearl whose surface will be modified) by this process, in particular when it is applied to a powder containing an inorganic pigment (mineral or synthetic) and / or a filler and / or a mother-of-pearl, made it possible to obtain a certain number of advantages, in particular in an ecodesign framework:

a simpler and inexpensive method of powder treatment comprising pigments and / or fillers and / or nacres, using a natural active ingredient (for example the raw ground material of a fruit or a seed , like the chestnut) and capable of achieving maximum functionalization of the powders without altering either the quality of the make-up powders or of this active ingredient; and - good skin hydration performance.

The subject of the present invention is a method for modifying the surface of a powder comprising a pigment, preferably mineral or synthetic, and / or a filler, and / or a nacre, said powder being intended to be used for the preparation of a cosmetic composition, characterized in that it comprises the following stages:

1) obtaining a ground vegetable, preferably a fruit or a seed, or seaweed, the ground being produced in aqueous solution;

2) bringing said powder into contact with said ground material, preferably with stirring;

3) filtration of the product obtained in step 2; and

4) drying the filtrate obtained in step 3.

By raw vegetable extract (or algae) is meant here to denote a raw extract of a fruit or of a seed which has not undergone a step of purification or concentration of an isolated active ingredient or of a molecule particular having the desired effect on the powder. A raw fruit or seed extract may be obtained before crushing from a fruit or seed which has preferably been peeled beforehand or from which the skins, the remains of the flower and / or the seeds to keep only the pulp, or from a flour of such pulp.

In step 1, the grinding can be carried out by any type of grinder, preferably by a knife mill, ball mill, hammer mill, air jet mill, roller press, mill tubes or even by a wheel mill.

In a particularly preferred embodiment of the present invention, said fruit, seed or alga is chosen from those containing carboxylic, phosphonic, amide, thiol or aromatic functions, preferably fruit or seed containing pectins and / or alpha- hydroxy acids, and said algae containing alginates.

For fruits containing pectins and their minimum concentration, one can refer for example to table 1 page 42 of the doctoral thesis of the University of Limoges (France) defended on July 16, 2007 by V. Brudieux

Preferably, said fruit or said seed is a fruit or a seed containing simple sugars (1 to 2 monomers), polysaccharides (number of monomers greater than 9) and polyols of the mono-, di-, oligo- or polysaccharide (see table 2).

Preferably, the fruit will be previously treated in order to remove its skin and, optionally, the seeds, so as to keep only the pulp.

In a particularly preferred embodiment, the fruit is chosen from chestnuts, bananas, apples, grapes, melons, apricots, hazelnuts, almond oil fruits, preferably chestnuts, moreover more preferred the chestnut from which the pericarp and the tan were previously removed.

For the composition of raw chestnut extracts, reference may also be made to document V. Brudieux (Doctoral Thesis, Univ. Limoges, France, defended on 2007-07-16), tables 6 and 7 on page 107 and tables 8 and 9 page 11, as well as, for the content of different sugars such as glucose, fructose and sucrose, in the JCM document Barreira et al. (Plant Foods Hum. Nutr. 2010, 65, p. 38-43, Tables 2 and 3)

Preferably, the fruits are fresh fruits, thawed fruits or even a flour obtained from the pulp of these fruits or seeds.

Also preferably, said cosmetic composition for which the powder is intended is a composition intended for making up or for cosmetic care of the skin, preferably intended for a foundation.

According to the present invention, said powder contains at least one pigment and / or a filler.

Advantageously, the method according to the invention is characterized in that:

step 1 of grinding comprises an acid or enzymatic hydrolysis of the ground material, preferably an acid hydrolysis. Preferably this step is carried out at a temperature between 20 ° C and 40 ° C if it does not involve the implementation of ultrasound (US); and or

- Step 1 of grinding includes a sonication step (passage to ultrasound), preferably this step 1 is carried out at a temperature of around 40 ° C (± 15%).

Acid hydrolysis can be carried out for example in the presence of sulfuric, hydrochloric acid, and at a pH greater than or equal to the pKa of pectins and preferably still lower than the isoelectric point (pHi) of the pigment or of the charge which it is desired to modify. the surface (for example, pHi of 6.6 for deTiO2), or preferably the acid hydrolysis is carried out at a pH such that:

pHi pigment / filler> pH> pKa pectin.

Even more preferably the pH is between 3.5 and 6.6, 3.5 and 5.5, or even more preferably between 4.0 and 5.0.

For acid hydrolysis, sulfuric, acetic, hydrochloric, oxalic acid or even carboxylic acids can be used, but not limited to.

The enzymatic hydrolysis can be carried out for example in the presence of enzymes (see for example the enzymes cited in the document of V. Durieux (2007) or also the apha-amylase, Alpha 1-6 glucosidase, maltase, beta galactosidase, beta glucosidase)

Advantageously also, the method according to the invention is characterized in that:

- Step 2 of contacting is carried out at a temperature between 40 ° C and 80 ° C with stirring, preferably between 60 ° C and 80 ° C; and or

- step 2 includes a sonication step if the latter has not been carried out in step 1.

Preferably, in step 3, filtration is carried out so as to remove particles larger than 200 μm in diameter, preferably greater than 150 μm (± 25%).

Preferably step 3 of filtration is carried out by sieving.

The preparation process of the invention comprises a drying step 4, the objective of which is to obtain a powder at the end of the process of the invention.

The removal of the volatile liquid (for example water) can be carried out with mechanical means such as suction, and / or by heat.

Those skilled in the art will know how to adapt the drying time necessary to optimize the elimination of the volatile phase. The powder in the end may include traces of more or less high volatile liquid. This proportion is preferably less than 2% by weight, more preferably less than 1% by weight relative to the total weight of the composition. It is generally sought to reduce as much as possible the proportion of residual volatile liquid in the final composition. The composition of the invention based on powders can be described as a “dry” powder, taking into account the very small residual amount of volatile liquid present in the end.

The drying may include a step consisting in exposing the product obtained in step 3 to a current of hot air, to infrared radiation to microwave radiation, or even in an oven.

In a preferred embodiment, in step 4, the drying is carried out by atomization or by lyophilization, preferably by atomization.

In a preferred embodiment of the invention, the percentage by weight of the raw vegetable or algae extract relative to the powder is between 5% and 20%, preferably between 7.5% and 15%, preferably 10%.

The pigments can be chosen from mineral pigments, organic pigments and pearlescent pigments.

Advantageously, said powder contains at least one pigment and / or a filler and said pigment preferably being an inorganic, mineral or synthetic pigment, preferably of mineral origin.

According to the present invention, said inorganic pigment is an inorganic pigment which can be composed of one of the following different chemical elements: F, Na, Mg, Al, Si, P, S, K, Ca, Ti, V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Zr, Mo, Ru, Cd, Sn, Sb, or W.

In a preferred embodiment, said inorganic pigment is a pigment chosen from mineral pigments or pearlescent pigments.

The mineral pigments can be chosen from metal oxides, preferably iron oxides, in particular black, yellow, red and brown iron oxides; manganese violet; ultramarine blue; chromium oxides, in particular hydrated chromium oxide, ferric blue, carbon black, and mixtures thereof.

The pearlescent pigments are for example chosen from mica coated with titanium oxide, mica-titanium coated with iron oxide, mica-titanium coated with chromium oxide or else mica-titanium coated with ferric blue.

The fillers can be chosen from mineral or organic fillers, preferably mineral.

Mention may preferably be made, but not limited to, charges such as:

- talc, preferably in the form of particles generally of dimensions less than 40 μm, preferably of the formula Mg3SÎ40io (OH) 2;

- Micas of natural or synthetic origin having dimensions from 2 to 200 μm, preferably from 5 to 70 μm and a thickness of 0.1 to 5 μm, preferably from 0.2 to 3 μm, more preferably the mica of formula X2Y4-6Zs02o (OH, F) 4 with

X = K, Na, Ca, Ba, Rb, Cs; Y = A1, Mg, Mn, Cr, Ti, Li and Z = Si, Al, Fe ³⁺ , Ti;

- kaolin preferably with particle sizes generally less than 30 pmn;

- the synthetic fluorphlogopite of formula KMg3 (AlSl30io) F2;

the sericite of formula KA1 ₂ [(OH, F) 2lAlSi ₃ Oio] / KA1 ₂ [(OH, F) ₂ IA1SÎ30io];

- silica of formula S1O2;

- Alumina of formula AI2O3 _;

- metallic soaps derived from organic carboxylic acids having from 8 to 22 carbon atoms, preferably from 12 to 18 carbon atoms, for example zinc stearate, magnesium stearate or lithium stearate, zinc laurate , magnesium myristate, preferably in the form of particles having dimensions less than 10 µm;

- zinc oxides, titanium oxides;

- calcium carbonate, magnesium carbonate, magnesium hydrocarbonate; and

- their mixtures

In a particular aspect of the invention, said pigment is a composite pigment formed from one or more inorganic pigments associated with one or more fillers, preferably chosen from the group consisting of the following composite pigments:

- Mica (43 to 87%) and T1O2 (13 to 57%);

- Mica (52 to 72%) and Fe ₂ O ₃ (28 to 48%);

- Mica (55 to 70%), TiO ₂ (28 to 38%) and Fe ₂ O ₃ (2 to 7%); and

- Mica (56 to 69%), TiO ₂ (10 to 28%), Fe ₃ O ₄ (1 to 12%), FeO (OH) (1 to 11%); Preferably, the powders (pigments and / or fillers) chosen from those in Table 1 below will be used:

Table 1

Metal oxides The charges White pigment: Micronized TIO2 (from 4.0 to 1.37 pm) in crystalline form: anatase and rutile. ZNO zinc oxide Colored mineral pigments: Iron oxide from yellow to black through red and brown. Manganese oxide (purple to pink) Chromium oxide III (green) The so-called colorless fillers: Talc Silica The micas. Calcium carbonates Light reflectors: Colorful muscovite-type micas. Synthetic micas: Fluorphlogopite

In another aspect, the subject of the present invention is a cosmetic composition comprising a powder containing pigments and / or a filler, preferably inorganic pigments, the surface of which has been modified by a surface modification method according to the present invention. .

The invention also relates to a cosmetic composition, the preparation of which involves the use of such a powder, the surface of which has been modified by a surface modification process according to the present invention.

Preferably, said cosmetic composition according to the invention is intended for making up or cosmetic care of the skin, preferably intended for the preparation of a foundation, an eyeshadow, a blush, a cream, a gel or a bar of soap, preferably a foundation.

In another aspect, the subject of the present invention is the use of a powder containing at least one pigment and / or a filler, said powder being mixed with a raw vegetable extract, preferably a raw extract of a fruit, d a seed or an alga chosen from those containing carboxylic, phosphonic, amides, thiols or aromatic functions, preferably fruits or seeds containing pectins and / or alpha-hydroxy acids, and said alga containing alginates, for the preparation of a cosmetic composition.

Preferably, the raw plant extract is a raw extract of chestnut from which the pericarp and the tan have been removed beforehand, or a flour obtained from such chestnuts.

More preferably, said powder contains at least one mineral pigment, preferably a metallic pigment.

In a last aspect, the invention relates to a foundation formulation, the composition of which comprises at least one or more pigments or fillers modified by a process according to the invention.

The following examples as well as the legends of the figures below illustrate the invention without however limiting it.

Legends of Figures

Figure 1: Diagram of a standard process for modifying the surface of a powder using a prior extraction of the active molecule of interest.

Figure 2: Diagram of the "Eco-Technological" process for modifying the surface of a powder using a crude extract of the active molecule of interest according to the invention.

Figure 3: Diagram representing the effects of a foundation obtained from a powder treated according to the invention on a skin section.

Figure 4 and Figure 5: Profile of the powder particle size (particle size) obtained with the method according to the invention according to the drying protocol used, by spraying (Figure 4) or by lyophilization (Figure 5).

Figure 6: Forearm areas tested according to the protocol used.

Figure 7: Residual effect of hydration after removing the powder obtained by the process of the invention according to Protocol 1 "Protocol 1 / ΊΊΟ2 / Atomization". Figure 8: Residual effect of hydration after removing the powder obtained by the process of the invention with Protocol 2 "Protocol2 (ETS) / TIO2 / Atomization". Figure 9: Residual effect of hydration after removal of the powder obtained by the process of the invention with Protocol 2 "Protocol2 (ETS) / TIO2 / Lyophilization".

Example 1: The metal oxides

Metallic oxides of titanium (white pigments) and iron (red, yellow and black pigments) for their coloring and opacity properties (coverage). We will also be interested in mineral fillers which are very widely used in cosmetics for their feel, their soft focus side and light reflector (see Table 1).

These compounds have very interesting physical properties from a sensory and visual point of view but are often very drying. This is due in part to the importance of their specific water-hungry surfaces provided by the many hydroxyl functions available. This development of specific surface will also give mineral powders absorbent powers of oils.

This peculiarity of mineral powders to bind with water molecules but also to absorb the oil causes when applied to the skin a feeling of dryness. Indeed, the hydrolipidic film of the skin will be immediately absorbed by the powders which will cause imbalances for certain skin types.

The fact of treating the powders used in make-up products on the surface will make it possible to reduce the available hydroxyl functions (OH) which react with the water contained in the stratum corneum and partly responsible for the drying of the seed coat. Thanks to this surface functionalization, the active ingredients essential for maintaining good skin hydration, such as polysaccharides, minerals and polyols, will be brought directly to the skin, thus making these powders biologically active (see Figure 3).

Operating principle of our surface treatment:

The present invention therefore consists in extracting fruit sugars (uronic acid) and their grafts in situ on the surface of the powders in one to two steps maximum, so as to contribute to sustainable development and to be part of an approach of eco extraction.

Indeed, the “classic” method would be to first extract the different carbohydrate fractions of the chestnut and to select only the “functional” part, before proceeding to the grafting of the carboxylic functions (COOH) on the surface of the powders. having hydroxyl (OH) functions available, wet. The dehydration step, on the other hand, is used to recover a functionalized and activated powder which will have better preservation.

The mechanisms of skin hydration

The cosmetic observatory in their article "Skin hydration, a layered approach: osmolytes" has been able to popularize the phenomena that allow the skin to maintain its hydration.

They highlighted three principles:

the dynamic circulation of water via aquaporins and intercellular spaces towards the surface, the retention of water by a stratified and well structured corneocyte barrier which limits perspiration, and finally the presence of polyols which, by hydrogen bonds , partially and locally capture the water molecules in transit.

Consequently, formulators will be able to work on their moisturizers by providing them with different categories of ingredients allowing them to play on these three principles.

Ingredient categories:

a) Film formers:

They remain on the surface of the skin and prevent perspiration of water or collect water molecules in transit.

Hydrophobic film-forming agent: hydrocarbons, vegetable oils, silicone oils, etc. Hydrophilic film-forming agent: hyaluronic acid, polysaccharides, cationic derivatives, etc.

b) Humectants:

They allow water to penetrate and retain at the level of the stratum corneum. Glycerin, sorbitol, synthetic glycol, urea, etc.

c) Osmolytes:

Their small sizes allow them to be transported by aquaporins to the heart of skin cells.

Carbohydrates of small sizes: mainly sugars.

Amino acids: glycines, etc.

Methyl amines: glycine betaines, etc.

Reading the previous paragraph on the skin's hydration mechanisms, we can observe that the dares (family grouping together sugars, polysaccharides, glucoaminoglycans, etc.) fall into three categories of ingredients that can play on skin hydration. .

Sugars: skin moisturizer

Sugars are present in the majority of plant elements in the form of simple sugars or a combination of sugar. It contains mainly glucose, fructose, but also xylose and sometimes sucrose. The more or less polymerized sugars are all considered as cosmetic active ingredients as cellular nutrients and moisturizers because they are part of the agents of NMF (Normal Moisturizing Factor).

Pectins are polysaccharides made up of a chain of alpha-D-galacturonic acid units linked together by bonds (beta-1,4), interrupted by the presence of L-rhamnopyranose units. Pectins are also powerful moisturizers for the skin because they are not hydrolyzed and fall into the category of hydrophilic film-forming agents. While once hydrolyzed they release their constituents which this time will behave like osmolytes and humectants.

Synergistic effect of the use of a raw plant extract according to the method of the invention (see Figure 2) compared to the standard use of a compound or active molecule previously extracted (see process of Figure 1)

Thus in view of the above, in order to have good hydration, it is necessary to find a balance between the film-forming agents, the humectants and the osmolytes. The crude extracts of the fruit all contain these three compounds in varying degrees, depending on the fruit, its variety and its maturity. Indeed, in fruits we have sugars such as:

polysaccharides (film-forming agents)

- polyols (humectants) simple sugars, free galacturonic acids and minerals (osmolytes) (see table 2)

Table 2

Table 1 - Structural classification of the main carbohydrates (1!

Class (DP) Subgroup Main compounds Sugars (1-2) Monosaccharides Glucose, galactose, fructose, tagatose Disaccharides Sucrose, lactose, trehalose, maltose Oligosaccharides (3-9) Malto-oligosaccharides Maltodextrins Other oligosaccharides Raffinose, stacchyose, verbascose, ajugose (a galactosides), fructooligosaecharides, galacto-oligosaccharides Polysaccharides (> 9) Starch Amylose, amylopectin, modified starches Non-starchy polysaccharides Cellulose, hemicelluloses (e.g. galactans, arabinoxylans), pectins, inulin, hydrocoids (e.g. guar) Hydrogenated carbohydrates (polyols) monosaccharide type Sorbitol, mannitol, xylîtol, erythritol disaccharide type isomalt, lactitol, maltitol oligosaccharide type Maltitol syrups, hydrogenated starch hydrolysates polysaccharide type Polydextrose (1) Source: AFSSA report (Carbohydrates and health: State of the piles, evaluation and recommendations, October 2004).

Unlike a raw plant extract from, for example, a fruit or a seed, a purified compound would provide the skin with only one of these three elements. The two other elements should therefore be added in order to have a formula with optimum hydrating power.

Another example proving the synergistic effect of elements contained in a fruit compared to an isolated and purified active principle is the example of vitamin C.

Example 2: Functionalization of T1O2 with active ingredients from the chestnut fruit a) Materials

Weigh: electronic balance at 0.01g and 0.001 precision

Crusher: with plunging head household appliances.

Ultrasoner: US Branson Digital Sonifier.

Shake: Magnetic stirrer combined with hot plate

Separation step: centrifuge, sieve at 160 micrometer.

Drying step: B-290 Sushi Atomizer

Characterize: Granulometer, TOC, pH meter.

Formula / Ingredients

Ingredients%

Chestnut, shelled and thawed 1% by weight

QSP 100 demineralized water

TIO2 9% (by weight)

Sulfuric acid at 2M qs

Protocol

Beforehand:

- Select the most beautiful chestnuts

- Shelled (remove the pericarp and the tan)

- Keep the almonds.

Step 1: Extraction of active molecules of interest

1 / In a suitable container weigh the chestnut, water and sulfuric acid. 2 / Grind everything: turbo speed / duration: 20 to 30 min.

3 / Put the container with the crushed chestnut in the US.

Setting :

amplitude 30% duration: 10min, 30s US pulses and 30s rest

T ° C 40 ° C

Step 2: surface treatment by liquid

4 / Introduce the TiO2 into the solution

5 / Heat the suspension to 60-70 ° C with stirring for 30 min. Step 3: Filtration

6 / Filter the solution through a 160 micron sieve *

Step 4: Drying

7 / Dry the solution with the B-290 bushi atomizer

Characterization of the powder obtained in step 4:

Determination of total organic carbon (TOC)

Sample preparation

1 / Passage of the suspension to the centrifuge 10,000 rpm, duration 5 min 2 / Dry the pellet in ambient air and grind it in mortar.

3 / Solid TOC analysis.

Example 3: Protocols for preparing the treated or functionalized pigments for carrying out an in-vivo test.

Objective: The aim of these tests is to validate the moisturizing effect of the powder that is functionalized or treated in-vivo according to different protocols.

Preparation of functionalized powders (tests on TIO2) with a view to demonstrating their hydrating effect by corneometric measurements (in-vivo test)

Preparation of the 15% Mother solution with and without the sonification step Table 3: Ingredients

Ingredients % Chestnut 15 Demineralized Water 85

Preliminary steps:

Defrost chestnuts

Shell the chestnuts and keep the almond

Weigh the almonds in order to obtain a 15% dispersion of chestnuts and make the QSP 100 with demineralized water

Grind the mixture (chestnut + water) with a plunge-head grinder for 20 min

Step A: Extraction of molecules of interest

Table 4: List of steps

Protocol 1 Protocol 2 Switch to ultrasound / duration 30 min / 1 Centrifuge 10,000 rpm for 5 min 1 2 Recover the supernatant and heat it to 60 ° C with stirring duration: 30 min 2 /

Measure to perform:

pH of chestnut crushed at 15% between 7 and 7.5 10 - pH of demineralized water = about 7

Step B: Surface treatment by liquid

Table 5: Ingredients

% Stock solution 15% chestnut 3 <X <5 TIO2 4 <Y <7 Water qs 100 Total 100

Weigh the ingredients under moderate agitation for 30 minutes

Drying step: recovery of the functionalized powder: We tested the drying process:

By atomization By Lyophilization

Granulometry of powders dried by atomization and of powders dried by lyophilization

The particle size profile clearly shows us that the addition of US in the protocol as well as the drying mode significantly influence the physical properties of the treated powders.

Comparative measurement by corneometry of the hydrating effect of functionalized powders on the epidermis according to the protocol

For these tests we want to compare the moisturizing effect of the different treatment processes carried out on ΊΊΟ2 compared to:

At ΊΊΟ2 without treatment

- A a B B Cream (Market reference)

Has a control zone

TIO2 and powders in general form an insulating layer. Therefore, it is difficult to measure hydration over time without removing the product.

It was therefore decided to adapt the standard protocol by removing the product after being in contact with the skin for several hours. The residual effect of our product is evaluated by measuring the hydration of the epidermis for several hours after the product has been removed (see Table 6).

Table 6

Type of study Comparative observational study for non-medical purposes on products under research and development. Adjustment of a standard hydration measurement protocol after application of emulsions, gels, to powders. Indications Cosmetic Highlight the residual effect by measuring the hydration of the epidermis for several hours after removing the product. Environment Study carried out on Montpellier in a closed room with a T = 22 ° C constant over the day. Product (s) studied 5.5 mg of untreated pigment TIO2 5.5 mg of sample 1 = ° Protocolel / TIO2 / Atomization 5.5mg of the sample2 = ° Protocol2 (US) / TIO2 / Atomization 5.5mg of the samples = ° Protocol2 (US) / TIO2 / Lyophilization 1ml of the B B cream market referent from Vichy Goal Evaluate the moisturizing effects on the forearms (5 treated areas) compared to a control area by comparing the initial state (T0) to the values after use at T1 (TO + 1h), T2 (T0 +

3h) and after removal of the products at T3 (TO + 4h + withdrawal), T4 (T3 + 1h), T5 (T3 + 3h) and T6 (T3 + 4h) by measurements of the hydration of the surface layers of the epidermis by coméometry on several subjects. Duration of the study 10 hours per observation. Fashion of use At the inner sides of the forearms: Before applying the product: delimitation of the 6 application areas. lh after the arrival of the subjects, application in each zone of the quantity by massaging until the product is homogeneous, the untreated zone serving as a control. Remove the product with water to dry the area and repeat the measurements after one hour. Criteria devaluation We must note and compare the measurements taken with the cormeometer on the treated areas. Methodology At the time of initial studies followed by application and withdrawal of the product: Tl (TO + 1h), T2 (TO + 3h), T3 (TO + 4h + withdrawal), T4 (T3 + lh), T5 (T3 + 3h) and T6 (T3 + 4h) Measurements of the hydration of the surface layers of the epidermis by impedancemetry with the CORNEOMETER CM825CK (at the level of the 5 treated zones and the control zone) according to the diagram presented in Figure 6

Results:

Sample 1 = ° Protocol 1 / TIO2 / Atomization Sample2 = ^o Protocol2 (US) / TIO2 / Atomization

Samples = ° Protocol2 (EiS) / TIO2 / Lyophilization

Observations and conclusion: (see Figures 7, 8 and 9)

We can therefore observe that on these three subjects, we do have a hydration higher than the control zone after the withdrawal of the samples. The residual effect is well observed.

We can also observe that it is sample 2 (Protocol2 (US) / TIO2 / Atomization) which obtains the best results.

The powder obtained after drying according to the process of the invention makes it possible to obtain the residual effect of hydration after the product has been removed.

The pigment thus treated is very biologically active since it hydrates even after the withdrawal of the product and this in the same way as a BB Cream.

Example 4: Liquid TOC Analysis Protocol

Analytical results highlighting the adsorption of molecules of interest on the surface of mineral pigments (ΊΊΟ2).

Preparation of the 10% mother solution

Defrost chestnuts

Shell the chestnuts and keep the almond

Weigh the almonds in order to obtain a 10% dispersion of chestnuts and make the QSP 100 with demineralized water

Grind the mixture (chestnut + water) with a plunge-head grinder for 20 min Table 7: ingredients

Ingredients % Chestnut 10 + 5 Demineralized Water 90 + 5

pH of chestnut chopped 10% = 7.3 pH of demineralized water = 6.95

Preparation of the extraction of active molecules of interest Code: 25012017.000 Work on 250 g (example)

Weigh the ground chestnut at 10% by weight of the total weight

Add demineralized water

Add a sufficient amount of sulfuric acid to (2M) so that the pH is> at pH3.5

Pass the dispersion to the US with the following parameters:

Amplitude 30%; Duration 10min; 30s US and 30s rest pits; T ° C 40 ° C Table 8: ingredients

Ingredients % Chopped chestnuts 10% 10 (i.e. 1% thawed chestnuts) Demineralized Water 90 Sulfuric acid (2M) qs (3.5 <pH <4)

Amplitude 30%; Duration 10min; 30s US and 30s rest pits; T ° C 40 ° C pH of the dispersion = 3.5

Liquid surface treatment

Preparation of samples for a liquid TOC measurement

The purpose of these tests is to prepare, from the same preparation (250,117,000), the tests with and without the introduction of TIO2 according to the protocol defined below.

Once the protocol has been completed, we perform a liquid TOC analysis (analysis of the supernatant) allowing us to account for the organic compounds adsorbed on the surface of the TIO2 compared to the tests which did not have contact with the white pigment.

For TOC analyzes) add centrifugation during the "Preparation of the extraction of active molecules of interest Code: 25012017.000" in order to eliminate the heterogeneity of the ground material. However, we will be far from the initial protocol because we would do the analysis as well as the treatment with the supernatant and not with the ground material.

Preamble:

In this protocol water is the solvent, it will then be eliminated.

There must be a relationship between the shelled fresh (or thawed) chestnut and the 1: 9 TIO2 (10% chestnut for 90% TIO2) before starting the manufacturing protocol for the functionalized pigment.

This protocol is written to perform a liquid TOC analysis.

Preparation of the functionalized powder:

Table 9: ingredients

Phase ingredients % Al Fresh or thawed shelled chestnuts 1 A2 Demineralized Water 99 A3 Sulfuric acid (2M) qs (3.5 <pH <4) B Mineral powder (TIO2) 9

Phase A: Extraction of molecules of interest

1 / In a suitable container weigh Al and A2.

2 / Grind Al and A2 for 20 min with a knife head chipper.

3 / Adjust the pH with A3, pH> 3.5

4 / Pass phase A (A1 + A2 + A3) under US with the following parameters:

Amplitude 30%; Duration 10min; Pits 30s US and 30s rest; T ° C 40 ° C.

5 / Filter the suspension with a filter at 160 micrometers. This step has been adapted to do the liquid TOC analysis.

6 / * Take (sample 1) with moderate stirring a sufficient amount of this phase for analysis with liquid TOC.

Phase B: Surface treatment by liquid

1 / Beforehand, adapt the quantity of phase B to be weighed (step 6 / phase A).

2 / Add phase B to phase A (A1 + A2 + A3) with moderate stirring.

The pH of B + A (A1 + A2 + A3) must be lower than the isoelectric point of the mineral powder so in the case of TIO2 the pH must be <6.6.

3 / Heat B + A (A1 + A2 + A3) according to the parameters:

Duration: lh; T ° C: 70 ° C; Moderate agitation.

4 / * Cool the dispersion and take a sample (sample 2) for the liquid TOC analysis.

5 / Atomize the suspension * Protocol for the liquid TOC analysis of samples 1 and 2:

Liquid TOC analysis:

This analysis was possible thanks to the expertise of Madame Azema, Professor at C2MA (Center des Matériaux des Mines d'Alès).

The competence of this research laboratory, belonging to the School of Mines of Alès, in the characterization of powders has enabled us to:

- To characterize the raw materials from a physico-chemical point of view.

- To validate the adsorption of organic molecules present in the chestnut on the surface of TIO2 (mineral powder).

Preparation of sample 1 (A1 + A2 + A3):

-1 / Heat the sample 1 / following the parameters:

Duration: hour; T ° C: 70 ° C; Moderate agitation

-2 / Pass the sample 1 / to the centrifuge:

Centrifugation speed: 10,000 rpm; Duration: 5 mins

-3 / Filter the supernatant with a 0.45 micrometer filter in a flask suitable for analysis with liquid TOC

Preparation of sample 2 B + (A1 + A2 + A3):

-1 / Pass the sample 2 / to the centrifuge:

Centrifugation speed: 10,000 rpm; Duration: 5 mins

-2 / Filter the supernatant with a 0.45 micrometer filter in a flask suitable for analysis with liquid TOC

Results interpretation :

Analyze the two samples with liquid TOC and compare them.

The result of the total organic carbon (TC) of the two samples must be different.

Fe total organic carbon (TC) expressed in [mg / 1] of sample 1 / must be greater than sample 2 /

Fa difference between ([mg / 1] of sample 1 / - [mg / 1] of sample 2) must be> 1 and it is this value which confirms the adsorption in [mg / 1] of the organic molecules of interest .

Result of the TOC analysis of the tests carried out after data processing, according to the protocol cited above:

Table 10: Results

Last name TC [mg / 1] TC average [mg / 1] Mean TC Difference [mg / 1] (Prevl- Prel2) Direct debit 1 600.62 610.28 73.76 Direct debit 1 619.94 Direct debit 2 526.46 536.52 Direct debit 2 546.59

Claims (19)

1. Method for modifying the surface of a powder comprising a pigment and or a filler, said powder being intended to be used for the preparation of a cosmetic composition, characterized in that it comprises the following steps: 1) obtaining a ground product of a fruit or a seed, the ground product being produced in aqueous solution; 2) bringing said powder into contact with said ground material; 3) filtration of the product obtained in step 2; and 4) drying the filtrate obtained in step 3. 2. Method according to claim 1, characterized in that the fruit or the seed is chosen from those containing carboxylic, phosphonic, amides, thiols or aromatic functions, preferably fruits containing pectins and / or alpha-hydroxy acids. 3. Method according to claim 2, characterized in that said fruit is the chestnut, preferably the chestnut from which the pericarp and the tan have been previously removed. 4. Method according to one of claims 1 to 3, characterized in that said cosmetic composition for which the powder is intended is a foundation. 5. Method according to one of claims 1 to 4, characterized in that said powder contains at least one pigment and / or a filler. 6. Method according to one of claims 1 to 5, characterized in that in step 1 of grinding is accompanied by a step: - hydrolysis, acid or enzymatic; and or -of heating, preferably between 40 and 80 ° C and / or; - passing through ultrasound. 7. Method according to one of claims 1 to 6, characterized in that in step 3, the filtration is carried out by sieving. 8. Method according to one of claims 1 to 7, characterized in that in step 4, the drying is carried out by atomization or by lyophilization, preferably by atomization. 9. Method according to one of claims 1 to 8, characterized in that percentage by weight of the plant or algae extract relative to the powder is between 7.5 and 15%. 10. Method according to one of claims 1 to 9, characterized in that said powder counteracts at least one pigment and / or a filler and in that said pigment is an inorganic pigment. 11. Method according to claim 10, characterized in that said inorganic pigment is an inorganic pigment which can be composed of one of the following different chemical elements: F, Na, Mg, Al, Si, P, S, K, Ca, Ti , V, Cr, Mn, Fe, Co, Ni, Cu, Zn, Se, Zr, Mo, Ru, Cd, Sn, Sb, or W. 12. Method according to claim 10 or 11, characterized in that said inorganic pigment is a pigment chosen from metal oxides, preferably chosen from TiO ₂ , ZnO, iron oxides, manganese oxides and chromium oxides. 13. Method according to one of claims 5 to 12, characterized in that said filler is chosen from excipients of natural or synthetic origin, preferably chosen from the following group: - Mica of formula X ₂ Y ₄ -6Z80 ₂ o (OH, F) ₄ with X = K, Na, Ca, Ba, Rb, Cs; Y = A1, Mg, Mn, Cr, Ti, Li and Z = Si, Al, Fe ³⁺ , Ti; - Synthetic fluorphlogopite of formula KMg3 (AlSl30io) F2; - Talc of formula Mg3Si ₄ Oio (OH) 2; - Sericite of formula KA1 ₂ [(OH, F) ₂ IAlSi ₃ Oio] / KA1 ₂ [(OH, F) ₂ IAlSi ₃ Oio]; - Silica of formula SiCh; - Alumina of formula AI2O3; and - Barium sulphate of formula BaSO ₄ . 14. Method according to one of claims 5 to 13, characterized in that said pigment is a composite pigment formed from one or more inorganic pigments associated with one or more fillers, preferably chosen from the group consisting of the following composite pigments: - Mica (43 to 87%) and TiO ₂ (13 to 57%); - Mica (52 to 72%) and Fe ₂ O ₃ (28 to 48%); - Mica (55 to 70%), TiO ₂ (28 to 38%) and Fe ₂ O ₃ (2 to 7%); - Mica (56 to 69%), TiO ₂ (10 to 28%), Fe ₃ O ₄ (1 to 12%), FeO (OH) (1 to 11%); -Fluorphlogopite synthetic (18 to 51%) and TiO ₂ (49 to 82%); and - Synthetic fluorphlogopite (23 to 48%) and TiO ₂ (52 to 77%). 15. Cosmetic composition comprising a powder, the surface of which has been modified by a process according to one of claims 1 to 14. 16. Cosmetic composition according to claim 15, for the preparation of a foundation, an eyeshadow, a blush, a concealer, a cream, a gel or a bar of soap, preferably a foundation. 17. Use of a powder containing at least one pigment and / or a filler, said powder being mixed with a raw plant extract, preferably a fruit, a seed or an alga chosen from those containing carboxylic, phosphonic, amide, thiol or aromatic functions, preferably fruit containing pectins and / or alpha-hydroxy acids, and said alga containing alginates, for the preparation of a cosmetic composition. 18. Use of a powder according to claim 17, characterized in that the crude plant extract is a crude extract of chestnut from which the pericarp and the tan have been previously removed. 19. Use of a powder according to claim 17 or 18, characterized in that said powder contains at least one mineral pigment, preferably a metallic pigment. Step 1 = extraction of active molecules of interest ...... ". , ÎSi ^{; i: ÎS} Plant selection Washing, grinding, etc. Extraction -> Maceration, enfleurage, etc. '''•your** 1/8