FR3134519A1 - NEW COMPOSITIONS COMBINING AT LEAST ONE INORGANIC SOLAR FILTER AND THEIR USE - Google Patents

Abstract

TITLE: NEW COMPOSITIONS COMBINING AT LEAST ONE INORGANIC SUNSCREEN AND THEIR USE The present invention relates to new compositions combining at least one inorganic sunscreen and their use in cosmetics, as well as their pharmaceutical use, in particular in dermatology, in particular as sun protection for the skin. (no figure)

Description

NEW COMPOSITIONS COMBINING AT LEAST ONE INORGANIC SOLAR FILTER AND THEIR USE FIELD OF INVENTION

The present invention relates to new compositions combining at least one inorganic sun filter and their use in cosmetics, as well as their pharmaceutical use, in particular in dermatology, in particular as sun protection for the skin.

STATE OF PRIOR ART

Exposure to solar radiation has beneficial effects, but during overexposure it can also cause deleterious consequences on the skin both in the short and long term, such as solar erythema known as "sunburn", accelerated aging of tissues, photodermatoses, even carcinomas or melanomas.

One of the main factors of skin aggression is considered to be ultraviolet solar radiation UV-A (λ = 320-400 nm) and UV-B (λ = 290-320 nm). UV-B radiation reaching the surface of the skin can cause, alongside tanning, burns and signs of aging. UV-A rays can penetrate deeper into the skin, causing the release of free radicals, causing changes in DNA. UV rays therefore have a pro-oxidant effect.

“Sunburn” or erythema induced by solar irradiation, or actinic erythema, clinically corresponds to histological characteristics marked by the presence of dyskeratotic cells or “ sunburn cells ”, corresponding to apoptotic keratinocytes. Actinic erythema is mainly linked to UV-B but also to the action of UVA. The consequences of UV-induced erythema are multiple, involving DNA damage, generation of reactive oxygen species (ROS), and an array of inflammatory mediators.

Natural photoprotection can be induced by the skin which has intrinsic defense systems allowing it to fight against the sun's aggressions. It is expressed by the production of photoprotective melanin pigments, or by a thickening of the stratum corneum with a greater number of layers of keratinocytes in the epidermis.

For prolonged or intensive exposure to solar radiation, photoprotection can also be induced and ensured by means such as the topical application of photoprotective cosmetic products such as sun creams. These products or preparations most often contain, solubilized or dispersed in an excipient, protective substances that can be classified into three main categories:

• physical filters, whose action aims to reflect all solar radiation and therefore prevent their penetration into the skin:
• chemical filters, whose action aims to absorb part of solar radiation, generally UV-A and UV-B radiation and then to release the photonic energy absorbed by thermal exchange with the skin:
• and finally so-called active photoprotective agents as opposed to filters, and which are generally substances capable of trapping reactive oxygen species ("ERO" or " ROS ") formed when radiation is absorbed by molecules naturally present in the skin (photosensitization mechanism).

More recently, other protection strategies have been developed with the introduction into sunscreen formulas of active agents such as DNA repair enzymes, peptides protecting DNA from UVA damage and antioxidant compounds. such as vitamins C and E, or polyphenols (Matsui MS et al ., J. Invest. Dermatol., 2009, vol.14, pp.56-59). Interest in this strategy has been reinforced by the recent demonstration of the capacity of visible (400-700 nm) and near infrared (700-1440 nm) radiation to also induce the formation of ROS in the skin (Liebel F. et al ., J. Invest. Dermatol., 2012, vol. 132, pp. 1901-1907: Schroeder P. et al ., Exp. Gerontol., 2008, vol. 43, pp. 629-632).

Such topical preparations are generally characterized by a sun protection factor "SPF" ( Sun Protection Factor ), indicator of the level of protection against solar erythema, adapted to particular sunlight conditions and skin phototypes. For high SPF sunscreen formulas, protective substances such as physical filters, chemical filters and photoprotective active agents are often combined. However, the combination of such heterogeneous active ingredients in topical formulas is not without problems: lack of stability, cost, biodegradability, formation in contact with oxygen, or its reactive species, of by-products including toxicology is often unknown.

High-performance chemical filters have been developed, presenting increased photostability and broad absorption spectra with respect to UV-A and/or UV-B. These chemical filters provide good photoprotection but their massive use is increasingly criticized because they often have allergenic properties and can be toxic or harmful if they penetrate through the epidermal barrier. Skin penetration of these soluble filters is a source of concern for their cumulative effects. Thus, several filters are suspected of being endocrine disruptors. In addition, filters are often poorly biodegradable and become environmental pollutants. Among other examples of ecotoxic effects, solar filters would have a negative impact on marine reefs and could contribute to the phenomenon of coral bleaching.

The general trend is therefore to limit the use of synthetic chemical filters.

Beyond these considerations, the sensory aspect for the user during the topical application of their preparations must also be taken into consideration.

The physical filters used in sun protection preparations are most of the time inert substances of mineral origin such as zinc oxide (ZnO) and titanium dioxide (TiO ₂ ) cerium oxide, oxide zirconium. Their use in sun protection products, however, remains difficult, with the appearance of white traces during application.

More than sixty phyto-cannabinoids are known, including non-psychotropic cannabinoids such as cannabidiol (CBD), cannabigerol (CBG), cannabinol (CBN), cannabichromene (CBC), cannabivarin (CBDV), cannabicyclol (CBL ) and cannabicitran (CBT).

By “phyto-cannabinoids” we mean cannabinoids of plant origin, that is to say from plants.

Thus, non-psychotropic phyto-cannabinoids contained in hemp such as cannabidiol and cannabigerol help relieve skin conditions such as inflammation and unexpectedly exhibit an attenuating effect on cell apoptosis induced by UV radiation. .

Other active substances such as biomimetic peptides can have a protective effect on the skin against solar radiation. Indeed, biomimetic peptides mimic the action of natural peptides, while being biocompatible. Among these biomimetic peptides, acetyl hexapeptide-1, an alpha-MSH agonist by stimulating melanin synthesis, helps reinforce the skin's natural photoprotection capacity by protecting it from DNA damage initiated by UV and reduces the appearance of solar erythema, soothes skin damaged by the sun and limits the signs of photoaging.

TECHNICAL PROBLEM

There is a need for topical application compositions to protect the skin against solar radiation and prevent its damage.

There is a need for topical compositions with strong sun protection with a texture allowing easy application and optimal coverage of the skin during application.

There is a need for topical compositions with strong sun protection which, after application, leave a feeling of hydration and softness and do not leave the sensation of a sticky film applied to the skin and do not leave unpleasant white marks on the skin.

There is a need for sun protection compositions limiting the use of chemical sun filters based on natural, biocompatible and non-toxic products, or based on environmentally friendly products.

One of the aims of the invention is to propose a combination of active substances making it possible to protect the skin against solar radiation, and in particular to prevent the ravages of prolonged exposure to the sun such as solar erythema.

Another aim of the present invention is to propose a combination of active substances making it possible to protect the skin against solar radiation based on natural products, including for example plant extracts, and/or based on biomimetic products, inspired by natural and biocompatible with the skin.

Another aim of the present invention is to propose a composition, in particular topical, comprising the association of different heterogeneous active substances, which is stable.

Another aim of the invention is to propose a topical composition which allows rapid and homogeneous application to the skin, transparency of the product after application and leaving on the skin a sensation of hydration and softness, without the sensation of a film applied to the skin.

A first object of the present invention is an association comprising or constituting a mixture of at least one zinc oxide, acetyl hexapeptide-1 and at least one non-psychotropic phyto-cannabinoid.

In a particular embodiment, the invention relates to an association as defined above, comprising or constituting a mixture of zinc oxide, acetyl hexapeptide-1 and a non-psychotropic phyto-cannabinoid.

In a particular embodiment, the non-psychotropic phyto-cannabinoid is chosen from the following group: cannabidiol (CBD), cannabigerol (CBG), cannabinol (CBN), cannabichromene (CBC), cannabivarin (CBDV), cannabicyclol (CBL) and cannabicitran (CBT).

In a particular embodiment, the invention relates to a combination comprising or constituting a mixture of zinc oxide, acetyl hexapeptide-1 and cannabidiol or cannabigerol.

Thus, among the different combinations of active substances for sun protection, the inventors have surprisingly observed that the association of a non-psychotropic phyto-cannabinoid, in particular cannabidiol (CBD) or cannabigerol (CBG), with acetyl hexapeptide-1 which is a stimulant of the natural production of melanin in the skin, and zinc oxide which is an inorganic filter, appears to have synergistic activity for the protection of the skin against solar radiation .

The inventors have obtained a topical composition comprising the combination of cannabidiol, with acetylhexapeptide-1 and zinc oxide having a creamy, stable and homogeneous texture facilitating penetration and coverage of the skin without leaving unsightly white marks. . The application of this composition gives a feeling of hydration, freshness and softness and not that of a film applied to the skin.

Cannabidiol (CBD) or 2-[(1R,6R)-6-isopropenyl-3-methylcyclohex-2-en-1-yl]-5-pentylbenzene-1,3-diol, is the second most common phyto-cannabinoid abundant in hemp. Cannabidiol can be extracted from several varieties of hemp, including Cannabis sativa , indica and ruderalis . In particular, it can be extracted pure from genetically modified hemp plants or synthesized in the laboratory. Its structure is presented below and it is a lipophilic substance and does not exhibit psychoactive effects.

Chemical structure of cannabidiol

CBD cannabidiol shows potential in reducing the skin's inflammatory response. Indeed, studies have shown that it has anti-inflammatory properties (Burstein S., Bioorganic & Medicinal Chemistry, Vol 23, 2015, p 1377-1385) and antioxidant properties (Booz G.W.: Free Radical Biology and Medicine, Vol 51, September 2011, p 1054-1061).

Cannabigerol (CBG) is another phyto-cannabinoid, present in low levels, around 1%, in hemp. Its structure is presented below.

Chemical structure of cannabigerol (CBG)

“Acetyl hexapeptide-1” is a biomimetic peptide mimicking the action of natural peptides which stimulate the synthesis of melanin. Acetyl hexapeptide-1 is a hexapeptide with the sequence “Ac-Nle-Ala-His-(D)Phe-Arg-Trp-NH ₂ ”. It is a biomimetic peptide (FR 2 835 528) of α-MSH. The structure of the molecule, whose CAS number is [448944-47-6], is presented above.

Chemical structure of Acetyl Hexapeptide-1

In a particular embodiment, the invention relates to an association as defined above comprising or constituting a mixture of zinc oxide, acetyl hexapeptide-1 and cannabidiol.

In a particular embodiment, the invention relates to an association as defined above, comprising or constituting a mixture of zinc oxide, acetyl hexapeptide-1 and cannabigerol.

In a particular embodiment, the invention relates to an association as defined above, comprising or constituting in a mixture:

• zinc oxide,
• acetyl hexapeptide-1,
• cannabidiol (CBD) and
• another non-psychotropic phyto-cannabinoid chosen from the group: cannabigerol (CBG), cannabinol (CBN), cannabichromene (CBC), cannabivarin (CBDV), cannabicyclol (CBL) and cannabicitran (CBT).

In a particular embodiment, the invention relates to an association as defined above comprising or constituting in a mixture:

• zinc oxide,
• acetyl hexapeptide-1,
• cannabidiol (CBD) and
• at least one other non-psychotropic cannabinoid chosen from the group cannabigerol (CBG), cannabinol (CBN), cannabichromene (CBC), cannabivarin (CBDV), cannabicyclol (CBL) and cannabicitran (CBT).

In a particular embodiment, the non-psychotropic phyto-cannabinoid is obtained according to the laws in force concerning the supply, use and marketing of such a product.

The cannabidiol and cannabigerol used can be of natural origin and come from plant extracts of different varieties of hemp, in particular Cannabis sativa, indica or ruderalis.

According to another particular embodiment, the cannabidiol or cannabigerol used comes from hemp extracts containing less than 0.3% THC, in particular less than 0.2% THC.

According to another particular embodiment, the cannabidiol or cannabigerol used is synthesized by methods known to those skilled in the art.

According to another particular embodiment, the acetyl hexapeptide-1 used is in the form of an oil.

Acetyl hexapeptide-1 can be presented in the form of a hydrophilic solution or as an oily, lipophilic dispersion/emulsion.

In oily form, it is marketed for example under the name MelinOil ^TM (INCI name: Isopropyl Palmitate (and) Lecithin (and) Water (and) Acetyl Hexapeptide-1 ) by the company Lucas Meyer Cosmetics). MelinOil ^TM from Lucas Meyer Cosmetics is a dispersion of acetyl hexapeptide-1 in a mixture of lecithin, isopropyl palmitate and water.

In aqueous form, acetyl hexapeptide-1 is marketed under the name Melitane ^TM (INCI name: Glycerin (and) Water (and) Dextran (and) Acetyl Hexapeptide-1 ). Melitane ^TM from Lucas Meyer Cosmetics is a solution of acetyl hexapeptide-1 in a mixture of glycerin, Dextran and water.

According to another particular embodiment, the zinc oxide used is in particulate form in a dispersant.

According to another particular embodiment, the zinc oxide dispersant used is chosen from: caprylic capric triglyceride, dicaprylyl carbonate, C12-15 alkyl benzoate and diisobutyl adipate.

A ZnO dispersion used is for example marketed under the name Xperse® 501 (INCI name: Zinc oxide (and) Caprylic/capric triglyceride (and) polyhydroxystearic acid ) from the company Evercare.

In a particular embodiment, the invention relates to an association as defined above further comprising titanium dioxide (TiO ₂ ).

In a particular embodiment, the invention relates to an association as defined above, comprising or constituting a mixture of zinc oxide, titanium dioxide, acetyl hexapeptide-1 and a non-psychotropic cannabinoid .

In a particular embodiment, the non-psychotropic cannabinoid is chosen from the following group: cannabidiol (CBD), cannabigerol (CBG), cannabinol (CBN), cannabichromene (CBC), cannabivarin (CBDV), cannabicyclol ( CBL) and cannabicitran (CBT).

In a particular embodiment, the invention relates to a combination as defined above, comprising or constituting a mixture of zinc oxide, titanium dioxide, acetyl hexapeptide-1 and cannabidiol or cannabigerol.

In a particular embodiment, the invention relates to a combination as defined above, comprising or constituting a mixture of zinc oxide, titanium dioxide, acetyl hexapeptide-1 and cannabidiol.

In a particular embodiment, the invention relates to a combination as defined above, comprising or constituting a mixture of zinc oxide, titanium dioxide, acetyl hexapeptide-1 and cannabigerol.

In a particular embodiment, the invention relates to an association as defined above further comprising:

• a solvent for acetyl hexapeptide-1,
• an emulsifier of acetyl hexapeptide-1,
• a zinc oxide dispersant,
• and water.

In a particular embodiment, the solvent for acetyl hexapeptide-1 is chosen from: isopropyl palmitate, glycerin, caprylic capric triglyceride, dicaprylyl carbonate and propanediol.

In a particular embodiment, the acetyl hexapeptide-1 emulsifier is chosen from: lecithin, sorbitan esters, alkyl polyglucosides and polyoxyethylene derivatives.

In a particular embodiment, the zinc oxide dispersant is chosen from: caprylic capric triglyceride, dicaprylyl carbonate, C12-15 alkyl benzoate and diisobutyl adipate.

In a particular embodiment, the invention relates to an association as defined above further comprising:

• a solvent for acetyl hexapeptide-1, in particular isopropyl palmitate,
• an emulsifier of acetyl hexapeptide-1, in particular lecithin,
• a dispersant of zinc oxide, particularly caprylic capric triglyceride
• and water.

In a particular embodiment, the invention relates to an association comprising or constituting in a mixture:

• zinc oxide,
• acetyl hexapeptide-1,
• cannabidiol or cannabigerol,
• a solvent for acetyl hexapeptide-1,
• an acetyl hexapeptide-1 emulsifier,
• a zinc oxide dispersant,
• and water.

In a particular embodiment, the invention relates to an association comprising or constituting in a mixture:

• zinc oxide,
• acetyl hexapeptide-1,
• cannabidiol,
• a solvent for acetyl hexapeptide-1,
• an acetyl hexapeptide-1 emulsifier,
• a zinc oxide dispersant,
• and water.

In a particular embodiment, the invention relates to an association comprising or constituting in a mixture:

• zinc oxide,
• acetyl hexapeptide-1,
• cannabigerol,
• a solvent for acetyl hexapeptide-1,
• an acetyl hexapeptide-1 emulsifier,
• a zinc oxide dispersant,
• and water.

In a particular embodiment, the invention relates to an association as defined above further comprising:

• titanium dioxide,
• optionally a titanium dioxide coating agent such as alumina, aluminum hydroxide, jojoba esters or stearic acid,
• possibly a support for the coating agent.

In a particular embodiment, the invention relates to an association as defined above further comprising:

• titanium dioxide,
• a titanium dioxide coating agent such as alumina, aluminum hydroxide, jojoba esters or stearic acid,
• a support for the coating agent.

In a particular embodiment, the invention relates to an association as defined above further comprising:

• titanium dioxide,
• optionally a titanium dioxide coating agent such as alumina, aluminum hydroxide, jojoba esters or stearic acid,
• optionally a support for the coating agent, in particular stearic acid or polyhydroxystearic acid dispersed in at least one surfactant, in particular chosen from polyglyceryl-2 Dipolyhydroxystearate and polyglyceryl-3 diisostearate.

In a particular embodiment, the invention relates to an association comprising or constituting in a mixture:

• zinc oxide,
• acetyl hexapeptide-1,
• cannabidiol or cannabigerol,
• titanium dioxide,
• a solvent for acetyl hexapeptide-1,
• an acetyl hexapeptide-1 emulsifier,
• a zinc oxide dispersant,
• possibly a titanium dioxide coating agent,
• possibly a support for the coating agent.
• and water.

In a particular embodiment, the invention relates to an association comprising or constituting in a mixture:

• zinc oxide,
• acetyl hexapeptide-1,
• cannabidiol,
• titanium dioxide,
• a solvent for acetyl hexapeptide-1,
• an acetyl hexapeptide-1 emulsifier,
• a zinc oxide dispersant,
• possibly a titanium dioxide coating agent,
• possibly a support for the coating agent.
• and water.

In a particular embodiment, the invention relates to an association comprising or constituting in a mixture:

• zinc oxide,
• acetyl hexapeptide-1,
• cannabigerol,
• titanium dioxide,
• a solvent for acetyl hexapeptide-1,
• an acetyl hexapeptide-1 emulsifier,
• a zinc oxide dispersant,
• possibly a titanium dioxide coating agent,
• possibly a support for the coating agent.
• and water.

In a particular embodiment, the invention relates to an association as defined above, in which:

• the zinc oxide in dispersion is present at a rate of 10% to 99% by total mass of the association,
• acetyl hexapeptide-1 is present at a rate of 1 ppm to 50 ppm, preferably 1 ppm to 10 ppm in total mass of the association, in particular 5 ppm, and
• cannabidiol or cannabigerol is present at a rate of 0.1% to 5%, preferably 0.25% to 1.5% as a percentage by total mass of the association.

In a particular embodiment, the invention relates to an association as defined above, in which:

• the zinc oxide in dispersion is present at a rate of 10% to 99% by total mass of the association,
• acetyl hexapeptide-1 is present at a rate of 1 ppm to 50 ppm, preferably 1 ppm to 10 ppm in total mass of the association, in particular 5 ppm, and
• cannabidiol is present at a rate of 0.1% to 5%, preferably 0.25% to 1.5% as a percentage by total mass of the association.

In a particular embodiment, the invention relates to an association as defined above, in which:

• the zinc oxide in dispersion is present at a rate of 10% to 99% by total mass of the association,
• acetyl hexapeptide-1 is present at a rate of 1 ppm to 50 ppm, preferably 1 ppm to 10 ppm in total mass of the association, in particular 5 ppm, and
• cannabigerol is present at a rate of 0.1% to 5%, preferably 0.25% to 1.5% as a percentage by total mass of the association.

The expression “0.1% to 5%” corresponds to the following ranges: from 0.1 to 0.5%: from 0.5 to 1.0%: from 1.0 to 1.5%: from 1 .5 to 2.0%: 2.0 to 2.5%: 2.5 to 3.0%: 3.0 to 3.5%: 3.5 to 4.0%: 4 0 to 4.5%: from 4.5 to 5.0%: and in particular approximately 0.5%.

The expression “from 0.25 to 1%” corresponds to the following ranges: from 0.25 to 0.50%: from 0.5 to 0.75%: from 0.75 to 1.0%: and in particular approximately 0.50%.

The expression "from 1 ppm to 50 ppm" corresponds to the following ranges: from 1 to 2 ppm: from 2 to 5 ppm: from 5 to 10 ppm: from 10 to 15 ppm: from 15 to 20 ppm: from 20 to 25 ppm: from 25 to 30 ppm: from 30 to 35 ppm: from 35 to 40 ppm: from 40 to 45 ppm: from 45 to 50 ppm: in particular around 5 ppm.

The expression “from 1 ppm to 10 ppm” corresponds to the following ranges: from 1 to 2 ppm: from 2 to 3 ppm: from 3 to 4 ppm: from 4 to 5 ppm: from 5 to 6 ppm: from 6 to 7 ppm: from 7 to 8 ppm: from 8 to 9 ppm: from 9 to 10 ppm: in particular around 5 ppm.

The expression “10% to 99%” corresponds to the following ranges: from 10 to 20%: from 20 to 30%: from 30 to 40%: from 40 to 50%: from 50 to 60%: from 60 to 70 %: from 70 to 80%: from 80 to 90%: from 90 to 99%.

In a particular embodiment, the invention relates to an association as defined above, further comprising titanium dioxide in dispersion present at a rate of 7 to 50%, by mass, preferably 10 to 49%.

The expression “7 to 50%” corresponds to the following ranges: from 7 to 15%: from 15 to 20%: from 20 to 30%: from 30 to 40%: from 40 to 50%.

In a particular embodiment, the invention relates to an association as defined above in which:

• the solvent for acetyl hexapeptide-1, in particular isopropyl palmitate, is present at a rate of 0.15% to 4% by total mass of the association,
• the emulsifier of acetyl hexapeptide-1, in particular lecithin, is present at a rate of 0.032% to 0.80% by total mass of the association,
• water is present at a rate of 0.008% to 0.20%, in total mass of the association.

In a particular embodiment, the invention relates to an association as defined above, further comprising:

• titanium dioxide dispersed in a suitable solvent, in particular caprylic capric triglyceride, present at a rate of from 7% to 50%, in total mass of the association,
• a first surfactant, in particular polyglyceryl-2 dipolyhydroxystearate, present at a rate of 1.5% to 5%, notably 2% to 4%, in total mass of the association
• a second surfactant, in particular polyglyceryl-3 diisostearate, present at a rate of 1.5% to 5%, notably 2% to 4%, in total mass of the association,
• optionally a titanium dioxide coating agent such as alumina, aluminum hydroxide, jojoba esters or stearic acid, present at a rate of 0.5% to 1.5%, by total mass from the Association,
• optionally a support for the coating agent, in particular in particular stearic acid or polyhydroxystearic acid dispersed in at least one surfactant, in particular chosen from polyglyceryl-2 dipolyhydroxystearate and polyglyceryl-3 diisostearate, present at a rate of 0.5% to 1.5%, in total mass of the association,

Another object of the present invention relates to a cosmetic composition comprising the combination as defined above which comprises or consists of a mixture of zinc oxide, acetyl hexapeptide-1 and cannabidiol or cannabigerol, in which said association is present at a rate of 10% to 60% by mass, preferably 15% to 25% by mass, in particular 20% by mass in a cosmetically acceptable medium.

By “ cosmetic composition ” is meant any composition for cosmetic purposes, in particular a composition which can be brought into contact with the superficial parts of the human body, the skin, in particular the epidermis, the mucous membranes and the scalp.

For the purposes of the present invention, the term “cosmetic composition” means a non-pharmaceutical composition, that is to say intended for skin which does not require therapeutic treatment, that is to say intended for any area of healthy skin.

The term "healthy skin" means an area of skin to which the association or composition according to the invention is applied, said to be "non-pathological" by a dermatologist, that is to say not showing infection, illness, or wounds or injuries and/or other dermatoses.

In a particular embodiment, the invention relates to a composition as defined above comprising the combination as defined above which comprises or consists of a mixture of zinc oxide, acetyl hexapeptide-1, of a non-psychotropic phyto-cannabinoid and titanium dioxide, in which said combination is present at a rate of 10% to 60% by mass, preferably 18% to 28% by mass, in particular 25% in a cosmetically acceptable medium .

By “a cosmetically acceptable medium ”, within the meaning of the invention is meant a medium compatible with use in cosmetics.

In a particular embodiment, the invention relates to a composition as defined above, said composition comprising at least one other cosmetic adjuvant or excipient, in particular chosen from: fatty substances, organic solvents, ionic or non-ionic thickeners , softeners, antioxidants, preservatives, emulsifiers, hydrophilic or lipophilic gelling agents, opacifiers, stabilizers, emollients, α-hydroxyacids, anti-foaming agents, moisturizing agents, vitamins, perfumes, preservatives, surfactants, fillers, sequestrants, polymers, propellants, alkalizing or acidifying agents, and dyes.

The composition may contain any other ingredient usually used in cosmetics, in particular for the manufacture of compositions intended for exposure to the sun in the form of emulsions.

Fatty substances may consist of an oil or wax or mixtures thereof, and they also include fatty acids, fatty alcohols and fatty acid esters. Fatty acid esters can be of plant origin (coconut, palm), or of synthetic origin.

The oils can be chosen from vegetable, mineral and synthetic oils, and in particular from petroleum jelly, polybutenes and isobutenes, isoparaffins and poly-α-olefins. Likewise, the waxes can be chosen from fossil, vegetable, mineral and synthetic waxes known per se, and beeswax.

The thickeners can be chosen in particular from crosslinked polyacrylic acids, and guar gums and celluloses modified or not such as hydroxy propylated guar gum, methylhydroxyethylcellulose and hydroxy-propyl-methylcellulose.

As “antioxidants”, we can cite, for example, tocopherol (vitamin E) or ascorbic acid (vitamin C).

As “preservatives”, we can cite, for example, benzalkonium chloride, phenoxyethanol, or sorbic acid.

As “emulsifiers”, we can cite, for example, polyol fatty acid esters, for example glycerol stearate, PEG-40 stearate, sorbitan Trèsstearate, polyoxyethylene sorbitan stearates (Tween®-60 or Tween®-20), ceteareth-20 (ethoxylated), cetyl alcohol.

As a “hydrophilic gelling agent”, we can cite, for example, carboxyvinyl polymers, acrylic copolymers, polysaccharides, natural gums, such as xanthan gum, clays, polyacrylamides.

As “lipophilic gelling agent” we can cite hydrophobic silica, clays modified with fatty chains.

Said adjuvants or excipients may be present in the composition in quantities conventionally used in cosmetics, in particular from 0.01 to 20% as a percentage by mass relative to the total mass of the composition.

In a particular embodiment, the invention relates to a composition as defined above, said cosmetic composition being formulated for topical application, in particular topical application of the skin, said composition being in particular in the form of an aerosol , an emulsion, a cream, a gel, a dispersion, a serum, a foam, a body milk or an anhydrous balm, preferably in the form of a body milk or cream.

Another object of the present invention relates to the use of a combination of the invention as defined above or of a cosmetic composition according to the invention as defined above as a protective agent from solar radiation (solar product ), in particular as sun milk.

Another object of the present invention is the use of an association according to the invention as defined above, or of a cosmetic composition according to the invention as defined above, in the cosmetic treatment of healthy skin. , particularly sensitive and/or reactive.

By “sensitive and/or reactive skin” we mean any skin subject to a feeling of discomfort which may manifest itself by more or less diffuse and localized redness, itching, tightness, irritation, burning sensations.

According to another particular embodiment, the present invention relates to the cosmetic use of an association according to the invention, or of a cosmetic composition according to the invention as defined above, in the cosmetic treatment of sensitive skin and/or or reactive.

For the purposes of the present invention, “cosmetic treatment” means a non-therapeutic treatment, that is to say intended for any area of healthy skin.

Another object of the present invention is a method of cosmetic treatment of healthy skin, in particular sensitive skin, comprising the topical application to healthy skin of an association according to the invention as defined above, or of a cosmetic composition according to the invention as defined above to reduce the sensations of tingling, tingling, itching or pruritus, burning, heating, discomfort or tightness of the skin.

For the purposes of the present invention, the term “cosmetic treatment method” means a method which does not require therapeutic treatment, that is to say a treatment method intended for any area of healthy skin.

According to another particular embodiment, the present invention relates to a method of cosmetic treatment, in particular of sun protection, for healthy skin, in particular sensitive skin, comprising an application of 1 to 5 times per day, in particular an application every two hours on a healthy skin.

According to another particular embodiment, the present invention relates to a method of cosmetic treatment, in particular sun protection, of erythema and inflammation of the skin due to exposure to the sun, comprising the application to the skin of an association according to invention, or a cosmetic composition according to the invention.

Another object of the present invention relates to a dermatological composition, comprising as active substance, an association according to the invention as defined above, with a pharmaceutically acceptable excipient,

said composition being particularly formulated for topical application, in particular topical application of the skin,

said composition being in particular in the form of an aerosol, an emulsion, a cream, a gel, a dispersion, a serum, a foam, a body milk or an anhydrous balm.

By “ dermatological composition ” is meant any composition for pharmaceutical purposes which can be brought into contact with the superficial parts of the human body, the skin, in particular the epidermis.

In a particular embodiment, the invention relates to a dermatological composition according to the invention as defined above, further comprising one or more active substances chosen from agents which fight against glycation, agents stimulating the synthesis of collagen or elastin or preventing their degradation, agents stimulating the synthesis of glycosaminoglycans or proteoglycans or preventing their degradation, anti-radical or anti-pollution agents, draining or detoxifying agents, desquamating agents, soothing agents and/or anti-irritants, astringent agents, agents acting on microcirculation, and mixtures thereof.

The list of active substances above is given in a non-limiting manner. The compositions according to the invention may also comprise one or more other additional active substances, the skilled person however ensuring that the possible complementary active compounds, as well as their proportions, are chosen in such a way that the advantageous properties recognized in the compositions according to the invention are not altered.

In a particular embodiment, the invention relates to a dermatological composition according to the invention as defined above, for its use for photoprotection against solar radiation.

Another object of the present invention relates to a process for preparing a composition comprising the combination of a mixture of zinc oxide, acetyl hexapeptide-1 and cannabidiol or cannabigerol comprising the following steps:

• a first step of preparing the aqueous phase A, said phase A comprising water, NaCl or MgSO ₄ , and propanediol, comprising the dissolution of the elements of phase A brought to temperature, in particular from 70 to 80 °C,
• a second step of introducing the elements of phase B, said phase B comprising cannabidiol, acetyl hexapeptide-1 and zinc oxide, optionally TiO ₂ , comprising:
• the introduction of cannabidiol, acetyl hexapeptide-1 and the other elements of phase B with deflocculating stirring, preferably from 800 to 1800 rpm, in particular for 10 min, preferably from 70 to 80°C, in the aqueous phase A, to form a clear solution,
• then the introduction of ZnO optionally with TiO ₂ with deflocculating stirring, preferably from 800 to 1800 rpm, in particular for 10 min, at a temperature of 70 to 80°C, in the aqueous phase A,
• then aspiration of the aqueous phase, in particular at 25 mL/min, with deflocculating stirring from 800 to 1800 rpm, giving a remaining solution in the form of an oily emulsion,
• maintaining stirring for 10 min at a temperature of 70-80°C and then maintaining stirring during the cooling phase of the remaining solution,
• optionally a step of introducing phase C, said phase C comprising perfumes or preservatives, at a temperature of approximately 40°C during the cooling step.

Particular embodiments of formulations according to the invention are given on a non-limiting basis.

The inventors have developed a formulation with the proportions indicated in Table 1. Said formulation comprises a mixture of Xperse® 501 comprising zinc oxide, Mélinoil ^TM comprising acetyl hexapeptide-1 and cannabidiol. The formulation in Table 1 can be used as an SPF30 sunscreen composition.

Phase Ingredients m/m% HAS Solvent -water QSP100 NaCl 0.50 Emollient 1 5.00 B Emollient 2 14.05 Emollient 3 4.00 CBD (crystal isolate) 0.25 Melinoil ^TM 0.50 Emulsifier 1 1.30 Emulsifier 2 3.00 Thickening agent 1.00 Antioxidant 0.05 Xperse® 501 33.00 Emollient 4 2.00 VS Scent 0.50 Conservative 1.00

Table 1. Formulation of an emulsion as SPF30 sunscreen

Another formulation developed by the Inventors is that with the proportions indicated in Table 2. Said formulation comprises a mixture of Xperse® 501 comprising zinc oxide, Mélinoil ^TM comprising acetyl hexapeptide-1, cannabidiol and of GranLux®TGL-50 including titanium dioxide. The formulation in Table 2 can be used in particular as an SPF50 sunscreen composition.

Phase Ingredients m/m% HAS Solvent water QSP100 NaCl 0.40 Emollient 1 2.50 B Emollient 2 11.55 Emulsifier 1 1.00 Emulsifier 2 2.00 Xperse® 501 23.70 GranLux® TGL-50 28.00 CBD (crystal isolate) 0.25 Melinoil ^TM 0.50 Antioxidant 0.10 VS Emollient 3 2.00 Scent 0.50 Conservative 1.00

Table 2. Formulation of an emulsion as SPF50 sunscreen

The following examples and figures illustrate the invention, without limiting its scope.

LIST OF FIGURES

There represents the UV absorption spectrum of an SPF30 sun cream according to the invention comprising ZnO, Melinoil ^TM and CBD.

There represents the UV absorption spectrum of an SPF50 sun cream according to the invention comprising ZnO, TiO ₂ , Melinoil ^TM and CBD.

EXAMPLES Example 1 – Composition of an SPF30 sunscreen

Phase Ingredients INCI m/m% HAS Distilled water/ Osmosis water Aqua/Water 33.20 NaCl sodium chloride 0.50 Cosphaderm® propanediol propanediol 5.00 B Cetiol® C5C BASF coco caprylate/caprate 14.05 Cetiol® CC Dicaprylyl carbonate 4.00 CBD (crystal isolate) cannabidiol 0.25 Melinoil ^TM isopropyl palmitate and lecithin and water and Acetyl Hexapeptide-1 0.50 Ensure + Pongamol/pongamia pinnata seed extract 0.25 Lameform® TGI BASF polyglyceryl-3 diisosteate 1.30 Dehymuls® PGPH BASF polyglyceryl-2 dipolyhydroxystearate 3.00 Compritol® 888 CG/DUB DBHG Glyceryl dibehenate 1.00 Natural Bisabolol Bisabolol 0.40 Tocopherol 70% non-GMO tocopherol 0.05 Xperse® 501 Zinc oxide and caprylic/capric triglyceride 33.00 Amihope® LL Lauroyl lysine 2.00 VS Scent perfume 0.50 Géogard® 221 dehydroacetic acid and benzyl alcohol and H ₂ O 1.00

Table 3. Composition of an SPF30 sun milk Example 2 – Preparation of an SPF30 sunscreen

The sun protection cream of Example 1 was prepared following the protocol described below.

In a beaker, the ingredients of the Phase A solution including water, NaCl chloride and propanediol were weighed separately and mixed forming a solution. The solution was stirred to dissolve the NaCl salt at a temperature of 72 to 75°C.

The ingredients of phase B were weighed and were introduced into the beaker to the solution of phase A, except the ingredient comprising ZnO (Xperse®501) and Lauroy lysine (Amihope®LL), under deflocculating stirring. , from 1000 to 1800 rpm for 10 min at a temperature of 75 to 80°C

The ZnO was then added with vigorous deflocculating stirring, from 1000 to 1800 rpm, for at least 10 minutes.

Lauroyl lysine was added with vigorous deflocculating stirring, from 1000 to 1800 rpm, for at least 5 minutes

The aqueous phase of the solution in the beaker was slowly sucked off while the solution was vigorously stirred from 1000 rpm to 1800 rpm.

The remaining solution was cooled.

The ingredients of phase C (perfume and preservative) were added one by one and mixed 5 minutes between each addition.

An emulsion in the form of a creamy, homogeneous and stable cream was obtained.

An emulsion stability test was carried out 24 hours after emulsion preparation.

The cream underwent a centrifugation test for 10 minutes at 3000 rpm (1600-1800 G) and retained its appearance of a homogeneous and stable emulsion.

Example 3: Composition of an SPF50 sunscreen

Phase Ingredients INCI m/m% HAS Distilled water/ Osmosis water Aqua/Water 25.85 NaCl Sodium chloride 0.40 Bio propane diol Propanediol 2.50 B Cetiol® C5C Coco-caprylate/caprate 11.55 Lameform® TGI Polyglyceryl-3 diisosteate 1.00 Dehymuls® PGPH Polyglyceryl-2 dipolyhydroxystearate 2.00 Xperse® 501 Zinc oxide and caprylic/capric triglyceride 23.70 GranLux® TGL-50 Titanium dioxide and caprylic/capric triglyceride and polyglyceryl-2 dipolyhydroxystearate and polyglyceryl-3 diisostearate and stearic acid and alumina 28.00 Ensure + Pongamol/pongamia pinnata seed extract 0.25 CBD (crystal isolate) Cannabidiol 0.25 Melinoil ^TM Isopropyl palmitate and lecithin and water and Acetyl Hexapeptide-1 0.50 Bisabolol Bisabolol 0.40 Bioxan® T Tocopherol 0.10 VS Amihope® LL Lauroyl lysine 2.00 Scent Perfume 0.50 Géogard® 221 Dehydroacetic acid and benzyl alcohol 1.00

Table 4. Composition of an SPF50 sun milk Example 4: Preparing an SPF50 sunscreen

The emulsion of Example 3 was prepared hot according to the protocol described below.

In a beaker, the ingredients of the Phase A solution including water, sodium chloride NaCl and propanediol were weighed separately and mixed. The solution was stirred to dissolve the NaCl salt at a temperature of 70 to 75°C.

The ingredients of phase B were weighed and were introduced into the beaker with the solution of phase A, except the ingredient comprising ZnO (Xperse®501) and that comprising TiO ₂ (GrandLux®, under deflocculating stirring). from 1000 to 1800 rpm for 10 min at a temperature of 75 to 80°C, forming a clear solution.

The ingredients comprising ZnO and TiO ₂ were then added with vigorous deflocculating stirring, for at least 10 minutes, while maintaining the temperature of 75 to 80°C.

The aqueous phase of the solution in the beaker was slowly sucked off while the solution was vigorously stirred from 800 rpm to 1800 rpm, for 10 minutes while maintaining the temperature.

The remaining solution was cooled while maintaining deflocculating agitation, from 800 rpm to 1800 rpm.

The ingredients of phase C were added one by one at a temperature of approximately 40°C.

An emulsion in the form of a creamy, homogeneous and stable cream was obtained.

An emulsion stability test was carried out 24 hours after emulsion preparation.

The cream underwent a centrifugation test for 15 minutes between 1500-2000 G and retained its appearance of a homogeneous and stable emulsion.

Example 5 – Sun protection evaluation method

Principle

The level of protection of a cosmetic product containing sun filters can be assessed by an in vitro spectrophotometric method.

The method allows you to provide:

- the “SPF” protection coefficient,

- the UVA protection factor “PF-UVA”, and

- the Critical Wavelength “LOC”, which must not be less than 370 nm, so that the formulated products can claim conformity of their UVA protection value, by a UVA logo.

To determine the effectiveness of sunscreen products, we evaluate their ability to prevent erythema that appears on the surface of the skin if it is exposed for a certain period of time to a source of UV energy. UVB represents only approximately 5% of the total UV energy received (UVA + UVB), but given their energy, they have a major effect on the appearance of this erythema. UVA, for their part, accounts for approximately 16% of the appearance of sunburn.

The method used consists of measuring the UV energy flow passing through the cream, expressed as energy transmission, and comparing this flow to the initial flow according to the principle of any spectrophotometric method: F(λ) = I / I0

Or :

• λ is the wavelength;
• I is the UV energy flux;
• I0 is the initial energy flow.

However, the comparison of these two curves is not sufficient to express the level of protection of the product spread on the skin. Indeed, two other wave functions are involved:

• The wave function of the source: In practice, this is the sun whose spectrum has been defined by the International Commission on Illumination as a wave function S(λ).
• The wave function concerning the skin: Cutaneous or subcutaneous reactions depend on the energy of the excitation light and are expressed in the form of a wave function E(λ).

By integrating each of these 3 curves over the entire UVB and UVA range and making the product of the 3 integrals, we will obtain the expression of the SPF In Vitro.

This method was initially described by B. Diffey and J. Robson (JSCC 40. 127-133 - 1989). It is today widely used and recognized by international authorities.

Materials and method

Laboratory equipment

• A UV spectrophotometer, Kontron 933 (BIO-TEK Kontron instruments) equipped with a UV source and a monochromator as well as an integrating sphere capable of delivering a UV energy flow between 290 and 400 nm. The wavelength increment is 1nm.

• A solar simulator, Suntest CPS+ (Atlas) to reproduce sunlight and take into account possible photodegradation of the tested sample.

The sample is spread on Sunplate polymethyl methacrylate (PMMA) plates (Helioscience), measuring 5 x 5 cm, having a rough phase obtained by sandblasting.

The tested product is spread according to the quantity recommended by the standards, i.e. 1.3 mg/cm ² for PMMA.

The sample is exposed to 2 minimum “MED” erythemal doses.

The MED value was chosen at 550 W/m ² , this value corresponding to exposure to zenithal sunlight. With this standard solar light, while receiving 2 MED, the product will therefore receive: 400 J/m ² .

The measuring device is calibrated beforehand with PMMA plates.

The tests are carried out on 3 PMMA plates on which the product is deposited. 4 measurements per plate were carried out with the spectrometer.

Determination of SPF value

The SPF in vitro is expressed from the entire residual UVB and UVA spectrum having passed through the layer of cream spread on the plate. However, this wave function T(λ) must be multiplied by:

• A first wave function which expresses the spectral characteristic of the sun S(λ).
• A second wave function which expresses the reactivity of the skin as a function of the wavelength (and therefore the energy dissipated): the erythematous function E(λ).

With :

• E(λ) is the action spectrum of erythema
• S(λ) is the standard solar spectrum
• T(λ) is the average transmission of the layer of the test product spread on an appropriate support
• d(λ) is the wavelength interval (1 nm)

Determination of the PF-UVA value

In vitro UVA protection is expressed from the entire residual UVA spectrum having passed through the same layer of cream.

With :

• P(λ) is the action spectrum of the PPD
• L(λ) is the spectrum of the Xenon arc lamp
• T(λ) is the average transmission of the layer of the test product spread on an appropriate support
• d(λ) is the wavelength interval (1 nm)

Determining the LOC value

In the calculation, λc corresponds to the wavelength for which the area under the absorption curve reaches 90% of the total area from 290 nm to 400 nm. The critical wavelength will therefore be determined according to the formula:

With :

• λc corresponds to the critical wavelength
• A(λ) corresponds to the absorption
• d(λ) corresponds to the wavelength interval between measurements

The critical wavelength λc of the product tested is obtained by calculating the arithmetic mean of the different measurements: all the selected measurements are taken into account for the calculation of the statistical dispersion.

Statistical expression of results

The average protection index of the preparation studied is obtained by calculating the arithmetic mean of the protection indices of each test.

The calculations are obtained using specific software which allows immediate access and without any manipulation to all the calculations necessary to obtain the values.

Example 6 – Protection tests of an SPF30 cream

The sun protection of the SPF 30 sun cream of the invention according to Example 1 was analyzed according to the method presented in Example 5. The results are reported in Table 5.

SPF
measure UVA LOC
n.m. SPF
Poster Sun milk SPF30
(ZnO, Melinoil ^TM , CBD) 37.0 20.1 374 30.0

Table 5: Protection analysis of an SPF 30 cream

As shown in the UV spectrum of the , the SPF30 sun milk of the invention according to the composition described in Example 1, has well-balanced protection, between UVB and UVA.

Example 7 – SPF50 protection tests

The sun protection of the SPF 50 sun cream of the invention according to Example 3 was analyzed according to the method presented in Example 5. The results are reported in Table 6.

SPF
measure UVA LOC
n.m. SPF
Poster Sun milk SPF50
(TiO ₂ , ZnO, Melinoil ^TM , CBD) 70.3 21.2 372 50+

Table 6: Protection analysis of an SPF 50 cream

As shown in the UV spectrum of the , the SPF50 sun milk of the invention according to the composition described in Example 3, has well-balanced protection, between UVB and UVA.

Claims (15)

Association comprising or constituting a mixture of zinc oxide, acetyl hexapeptide-1 and cannabidiol or cannabigerol. Association according to claim 1, further comprising titanium dioxide. Association according to claim 1, further comprising:

• a solvent for acetyl hexapeptide-1, in particular isopropyl palmitate,
• an emulsifier of acetyl hexapeptide-1, in particular lecithin,
• a dispersant of zinc oxide, in particular caprylic capric triglyceride
• and water.

Association according to claim 3, further comprising:

• titanium dioxide,
• optionally a titanium dioxide coating agent such as alumina, aluminum hydroxide, jojoba esters or stearic acid,
• optionally a support for the coating agent, in particular stearic acid or polyhydroxystearic acid dispersed in at least one surfactant, in particular chosen from polyglyceryl-2 Dipolyhydroxystearate and polyglyceryl-3 diisostearate.

Association according to one of claims 1 to 4, in which:

• the zinc oxide in dispersion is present at a rate of 10% to 99% by total mass of the association,
• acetyl hexapeptide-1 is present at a rate of 1 ppm to 50 ppm, preferably 1 ppm to 10 ppm in total mass of the association, in particular 5 ppm, and
• cannabidiol or cannabigerol is present at a rate of 0.1% to 5%, preferably 0.25% to 1.5% as a percentage by total mass of the association.

Association according to claim 5, further comprising titanium dioxide in dispersion present in an amount of 7 to 50%, by mass, preferably 10 to 49%. Cosmetic composition comprising the combination according to one of claims 1, 3 and 5, in which said combination is present in an amount of 10% to 60% by weight, preferably 15% to 25% by weight, in particular 20% by weight. mass in a cosmetically acceptable environment. Cosmetic composition comprising the association according to one of claims 2, 4 and 6, in which said association is present in an amount of 10% to 60% by mass, preferably 18% to 28% by mass, in particular 25% in a cosmetically acceptable environment. Cosmetic composition according to one of claims 7 or 8,
said composition comprising at least one other cosmetic adjuvant or excipient, in particular chosen from: fatty substances, organic solvents, ionic or non-ionic thickeners, softeners, antioxidants, preservatives, emulsifiers, hydrophilic or lipophilic gelling agents, opacifiers, stabilizers, emollients, α-hydroxy acids, anti-foaming agents, moisturizing agents, vitamins, perfumes, preservatives, surfactants, fillers, sequestrants, polymers, propellants, alkalizing agents or acidifiers, and colorings. Cosmetic composition according to one of claims 7 to 9, said cosmetic composition being formulated for topical application, in particular topical application of the skin, said composition being in particular in the form of an aerosol, an emulsion, an anhydrous cream, gel, dispersion, serum, foam, body milk or balm, preferably in the form of a body milk or cream. Use of an association according to one of claims 1 to 6 or of a cosmetic composition according to one of claims 7 to 10 as sun milk. Dermatological composition, comprising as active substance, an association according to one of claims 1 to 6, with a pharmaceutically acceptable excipient,
said composition being particularly formulated for topical application, in particular topical application of the skin,
said composition being in particular in the form of an aerosol, an emulsion, a cream, a gel, a dispersion, a serum, a foam, a body milk or an anhydrous balm. Dermatological composition according to claim 12,
further comprising one or more active substances chosen from agents which fight against glycation, agents stimulating the synthesis of collagen or elastin or preventing their degradation, agents stimulating the synthesis of glycosaminoglycans or proteoglycans or preventing their degradation, anti-radical or anti-pollution agents, draining or detoxifying agents, desquamating agents, soothing and/or anti-irritant agents, astringent agents, agents acting on microcirculation, and mixtures thereof. Dermatological composition according to one of claims 12 or 13, for its use for photoprotection against solar radiation. Process for preparing a composition comprising the combination of a mixture of zinc oxide, acetyl hexapeptide-1 and cannabidiol or cannabigerol, comprising the following steps:

• a first step of preparing the aqueous phase A, said phase A comprising water, NaCl or MgSO ₄ , and propanediol, comprising the dissolution of the elements of phase A brought to temperature, in particular from 70 to 80 °C,
• a second step of introducing the elements of phase B, said phase B comprising cannabidiol, acetyl hexapeptide-1 and zinc oxide, optionally TiO ₂ , comprising:
• the introduction of cannabidiol, acetyl hexapeptide-1 and the other elements of phase B with deflocculating stirring, preferably from 800 to 1800 rpm, in particular for 10 min, preferably from 70 to 80°C, in the aqueous phase A, to form a clear solution,
• then the introduction of ZnO optionally with TiO ₂ with deflocculating stirring, preferably from 800 to 1800 rpm, in particular for 10 min, at a temperature of 70 to 80°C, in the aqueous phase A,
• then aspiration of the aqueous phase, in particular at 25 mL/min, with deflocculating stirring from 800 to 1800 rpm, giving a remaining solution in the form of an oily emulsion,
• maintaining stirring for 10 min at a temperature of 70-80°C and then maintaining stirring during the cooling phase of the remaining solution,
• optionally a step of introducing phase C, said phase C comprising perfumes or preservatives, at a temperature of approximately 40°C during the cooling step.