EP3125951A1

EP3125951A1 - Method for processing cosmetic products under high hydrostatic pressure, products obtained and suitable container

Info

Publication number: EP3125951A1
Application number: EP15725707.2A
Authority: EP
Inventors: Gérard Demazeau
Original assignee: HPbiotech
Current assignee: HPbiotech
Priority date: 2014-03-31
Filing date: 2015-03-31
Publication date: 2017-02-08
Also published as: FR3019046A1; CN106456810A; WO2015150693A1; FR3019046B1; US20170106107A1

Abstract

The subject matter of the invention is a method for processing a cosmetic product with high hydrostatic pressures, consisting of applying a pressure P to the cosmetic product, with a continuous or cyclic application mode MA. It is characterised by at least one, and preferably all, of the following parameters: - a total application time t of pressure P of between 2 and 60 minutes, - a pressure P of between 200MPa and 600MPa, - a pressure application speed, for a compression VA, of between 1 and 5QMPa/s, - a decompression speed VAp of between 1 and 50 MPa/s, - when the application mode is cyclic, a latency time tiat applied before the first cycle and/or between certain cycles and/or between each cycle, - an initial temperature of between -10°C and 40°C. The invention also concerns the use of this method to deactivate at least one microorganism present in the pharmaceutical product or to modify the texture of same, and the cosmetic product obtained and a device suitable for implementing same.

Description

PROCESS FOR TREATING COSMETIC PRODUCTS

UNDER HIGH HYDROSTATIC PRESSURES,

PRODUCTS OBTAINED AND CONTAINERS ADAPTED

The present invention relates to a process for the treatment of cosmetic products by high hydrostatic pressure, in particular to irreversibly inactivate pathogenic microorganisms that can contaminate them while preserving their properties. The invention also relates to the products obtained and a container adapted for the treatment of cosmetic products and their preservation after treatment.

Cosmetic products are sensitive products that can be contaminated by certain microorganisms. In order to avoid any health problem, especially in contact with the skin in the case of cutaneous use, it is necessary to decontaminate these products. Various techniques have been described for this purpose: thermal techniques such as pasteurization and possibly sterilization, ionizing radiation treatment techniques, and more recently other physical techniques such as ultrasound or microwaves. However, all these processes, especially through the developed energy, can lead to an alteration of the intimate structure of the processed cosmetic products (destabilization of emulsions, free radical formation, etc.) and therefore of their intrinsic properties.

Moreover, in order to avoid any proliferation of residual microorganisms in cosmetic products treated with the abovementioned processes or in untreated cosmetic products, it is necessary to resort to the use of agents known as "preservatives", having either a bactericidal effect or effects limiting microbial growth. However, in recent years, various regulations limit the use of some of these preservative additives. In addition, in the case of products with the "Bio" label, these chemical preservatives change the image of neutrality associated with these products.

Also, there remains an important need for a process overcoming the disadvantages of the prior methods, in particular to sterilize a cosmetic product and allow its conservation without resorting to chemical additives, while retaining its characteristic properties.

It is the objective of the present invention to respond to this proposes a treatment method based on high hydrostatic pressure (HHP) technology.

HHP processes are known for the treatment of certain media. In particular, it has been shown that the application of HHP on food products can lead to reduce the microbial load (yeasts, molds, bacteria ...) and thus allow an increase in their shelf life (E. RENDUELES et al., "Microbiological Food Safety Assessment of High Hydrostatic Pressure Processing: A Review," LWT-Food Science and Technology (2011), 44, pp. 1251-1260). However, it must be emphasized that the inactivation conditions of these microorganisms depend both on the nature of the microorganism (for example the nature of the strain) and the composition of the medium. In particular carbohydrates, proteins, lipids and other constituents (salt and sugar concentrations ...) can have a protective effect for microorganisms vis-à-vis the effects of high pressure (JC CHEFTEL "Review: High Pressure, Microbial Inactivation and Food Preservation," Food Science and Technology International (1995), 1 (2-3) at 75-90, C. GARCIA-GRAELLS et al., "Inactivation of E. coli in milk. by high hydrostatic pressure treatment in combination with antimicrobial peptides, J. Food Prot (1999), 62, pp. 1248-1254). In parallel, certain physicochemical properties of the treated medium can have a strong impact on the pressure sensitivity of the microorganisms, in particular the pH value and the value of the water activity aw (JPPM SMELT "Recent Advances in the Microbiology of High Pressure Processing ", Trends Food Sci Technol., (1998, 9, pp. 152-158) The inactivation of microorganisms by the application of HHP is therefore a complex phenomenon since strongly dependent on many factors characteristic of the environment treated.

Thus, microbial inactivation by a HPP method in various cosmetic media often rich in lipids (for example emulsions of an oily phase in an aqueous phase or an aqueous phase in an oily phase) or containing polysaccharides , appeared until today hardly accessible.

In addition, certain cosmetic products of fragile nature such as emulsions, have an intimate structure that can be altered by applying high pressures because of their metastable nature (from a thermodynamic point of view). Nevertheless, surprisingly, thanks to the specific combination of particular parameters which act synergistically, the invention consists of a HHP treatment process for cosmetic products which makes it possible to sterilize them and irreversibly inactivate the pathogenic microorganisms that to contaminate them without using any preservative-type additive and while retaining their characteristic properties.

In particular the invention relates to a method for treating a cosmetic product by high hydrostatic pressure, consisting in applying a pressure P to the cosmetic product, with a continuous or cyclic mode of application MA, characterized by a speed VA of application of the pressure P for the compression between 0.5 and 50 MPa.s ^-1 , and at least one of the following parameters, preferably all:

o a decompression rate of between 0.5 and 50 MPa.s ¹ ,

a total duration t of application of the pressure P of between 2 and 60 minutes,

a pressure P of between 200 MPa and 600 MPa,

an initial temperature of the cosmetic product to be treated between -10 ° C. and 40 ° C.

Advantageously, such a method makes it possible to decontaminate the cosmetic products treated by irreversibly inactivating pathogenic microorganisms that can contaminate them, while retaining their intrinsic properties.

The invention also relates to the uses of this process, in particular for sterilizing cosmetic products, and the cosmetic products obtained.

Finally, the invention also provides a device adapted to contain products to be treated and treated by high pressure, in particular cosmetic products.

The invention is now described in detail, the description of the device being established with reference to the accompanying drawings, drawings in which the different figures show:

Figure 1: Schematic sectional view of a flexible envelope operculum.

Figure 2: Schematic sectional view of an over-container for receiving the flexible envelope.

Figure 3: Schematic view of a dispenser cap.

- Figure 4: Schematic view of the elements of Figures 1-3, assembled.

The invention therefore relates to a method for treating a cosmetic product by high hydrostatic pressure, comprising applying to the cosmetic product a pressure P, with a continuous or cyclic MA application mode. Preferably, the mode of application is cyclic.

By "cosmetic products" within the meaning of the invention is meant both:

finished product cosmetic compositions for application to the skin, mucous membranes or integuments, and

the constituents of these compositions, in particular the active cosmetic ingredients and the additives or excipients, for example plant extracts or floral waters.

"Cosmetic products" may be in any form suitable for treatment with HHP, that is to say in any form likely to lead the pressure, in particular creams, ointments, serums, lotions, water-based products floral, emulsions and certain powders having a surface treatment and grain size suitable and known to those skilled in the art to reduce the effects of compaction.

The method of high hydrostatic pressure according to the invention is characterized by a number of parameters, in particular:

the value of the pressure P,

the speed of application of the pressure for the compression VA,

- the speed of decompression VA and can be identical or different,

- the mode of application of the MA pressure, which represents the way it is applied during the treatment: either continuously with the same value of the pressure throughout the duration of the treatment once the desired value is reached, or cyclic way,

the initial temperature Ti of the cosmetic product to be treated,

the total duration t of application of the pressure P for the process.

The pressure P of the process according to the invention is between 200 MPa and 600 MPa.

The speed VA of application of the pressure P for the compression is between 0.5 and 50 MPa.s ^-1 , and preferably the speed VAn of decompression is between 0.5 and 50 MPa.s ^-1 .

Preferably, the process has a total duration t of application of the pressure P of between 2 and 60 minutes.

The initial temperature Ti of the cosmetic product to be treated is preferably between -10 ° C. and 40 ° C. According to a particularly suitable embodiment, the invention relates to a process for treating a cosmetic product by high hydrostatic pressure, consisting in applying a pressure P to the cosmetic product, with a continuous or cyclic, preferentially cyclic, mode of application MA, characterized by at least all of the following parameters:

a pressure P of between 200 MPa and 600 MPa,

an application velocity VA of the pressure P for the compression between 0.5 and 50 MPa.s ^-1 ,

o a decompression rate of between 0.5 and 50 MPa.s ^-1 ,

an initial temperature Ti of the cosmetic product to be treated between 10 ° C. and 40 ° C.

In the case of a cyclic application the process consists of a series of cycles. A cycle is described by a rise in pressure with the speed VA, a maintenance of the pressure at the value P for a duration then a descent in pressure with a speed

:

- up to the ambient pressure

- up to an intermediate pressure between ambient pressure and higher pressures P applied during said two cycles.

The duration of application of the pressure P of each cycle is preferably between 2 and 20 minutes, preferably between 3 and 15 minutes. Either all the cycles have an identical duration, or at least two cycles have a duration different.

Similarly, the pressure P may be identical for all the cycles or for at least two of the cycles the applied pressure P is different.

The compression speed VA and / or decompression can be identical for

all cycles or at least two of the cycles have a different compression speed VA and / or decompression. In some cases, for particular products, it is

necessary to apply a specific compression or decompression profile characterized in that the speed VA or may vary.

Indeed, each cycle has a profile of compression and decompression. The compression or decompression profile corresponds to the general appearance of the application of the pressure during ascent or descent. Thus, the compression and decompression can be monotonous (at constant speed or with variable speeds) or with one or more pressure levels. Each bearing is made by applying an intermediate constant pressure of a value between the lowest pressure of the cycle and the highest pressure of the cycle. The achievement of this or these bearing (s) can be done at constant speed or at variable speeds. Before and after each step, the speed of application may be the same or different.

Also, according to one embodiment, for at least one cycle, the compression speed VA and / or the decompression speed varies until the pressure P is reached.

cycles have the same profile of compression and / or decompression or at least two cycles have a different compression profile and / or decompression.

Moreover, for the same cycle, the compression profile and the decompression profile may be identical or different, that is to say that for the same cycle the speeds VA and may be identical or different.

Latency can be applied before the first cycle and / or between certain cycles

and / or between each cycle: either at ambient pressure or at intermediate pressure

This latency time is between 2 and 20 minutes. According to an embodiment

in particular, the method comprises at least three cycles, and at least one latency

If there are at least two latency times these latency times may be the same or

different.

The total duration of application of the pressure P for the process is between 2 and 60 minutes. It is dependent in the case of a cyclic MA application, the number of cycles and the duration of each cycle at the treatment pressure P, the duration of the time of

latency of VA speeds and

The number of cycles depends on the barosensitivity of the microorganisms to be inactivated and the treated cosmetic medium thus induces the total duration of maintenance t under high pressures. This number of cycles can not exceed 15 cycles.

The initial temperature Ti of the medium is -10 ° C to 40 ° C. This temperature can be the ambient temperature (20 to 25 ° C) or a lower temperature or a negative temperature or a higher temperature. Low temperatures (below 10 ° C) and negative temperatures are well suited to very fragile cosmetic products (such as those containing thermolabile active ingredients) because they make it possible to preserve the Specific characteristics and the higher temperatures of between 30 and 40 ° C make it possible to ensure very good inactivation of the spores when the cosmetic product contains them.

The compression speed, that is to say the rate of rise of the pressure, is between 0.5 and 50M Pa.s ^-1 , in particular between 1 and 50 MPa.s ^-1 . Preferably it is between 1 and 10 M Pa.s ^-1 , even more preferably between 1 and 6.6 MPa.s ^-1 . This speed can be constant or variable until the desired pressure is reached. Similarly, for two different cycles, the compression speed may be the same or different.

The decompression rate, that is to say the rate of descent of the pressure, is between 0.5 and 50 MPa.s ^{-1, in} particular between 1 and 50 MPa.s ^-1, preferably between 1 and 50 MPa.s ^-1 . and 10 MPa.s ^-1 , even more preferably between 1 and 6.6 MPa.s.sup.- ^1, This speed can be constant or variable until the desired pressure is reached.Also, for two different cycles, the decompression rate can be identical or different.

For the same cycle, or when the application mode of the pressure MA is continuous, the compression and decompression speeds may be identical or different.

The method is implemented using "high pressure" devices adapted to the conditions of the invention.

In order to avoid any subsequent contamination after the HHP treatment, the cosmetic product to be treated must be preconditioned in its final packaging or part of its final packaging. This packaging must:

o be completely or partially deformable, in order to be able to transmit the pressure, that is to say so that the application of the pressure can compensate for the compressibility of the treated cosmetic medium,

o not be altered by the application of HHP treatment, that is to say that it must have adequate mechanical strength, chemical integrity and barrier properties,

o preferentially not to bring contamination of the product during its use by the consumer, such as in particular "single-dose" type systems or any system avoiding a re-contamination by returning a little product or air in the packaging- tank. For example, it may be a packaging made of rigid material such as glass, plastic or any other suitable material to be used as a container, closed by a deformable seal or having a deformable part.

The cosmetic products thus packaged are then placed in a high pressure equipment and this equipment called "high pressure chamber" is closed by at least one shutter ensuring tightness. There is usually only one shutter when the "High Pressure" speaker is in the vertical position and there are usually two shutters (one at each end) when the speaker is in the horizontal position.

The pressure is transmitted to the samples by a liquid that does not alter the packaging during the treatment with the HHP process according to the invention. In some cases, a gas can be used to save the packaging (especially airless type).

The pressure increase can be achieved either with one or more pumps (in this case, the volume of the enclosure "High Pressures" is generally constant), or by reducing the volume of the enclosure.

The various parameters characterizing the HHP treatment to be applied are entered on a PLC or computer (according to the data transmission system to the equipment). Once the treatment is complete, the "High Pressure" chamber is opened and the samples are recovered. In the case where the cosmetic product has been treated directly in its final packaging (marketing packaging) it can be either repackaged in an overpack, or stored or sent to customers. In the case where the packaging is a part of the final packaging it is then associated with the various elements of said final packaging.

It is possible to treat the outer surface of the package or to select the outer layer of this package to avoid any wetting effect by the liquid used as a pressure transmitter medium.

According to a particularly suitable variant, the cosmetic product is packaged in a specific device, which allows both to apply the method according to the invention and to preserve the product after treatment.

This device for applying a high pressure process, in particular the method according to the invention, to a product, in particular to a cosmetic product, can take the following form. In Figure 1 there is shown a flexible reservoir shell 10 with an opening 11 in the upper part. A product 12, in this case a cosmetic product, is introduced into this envelope by any known means such as a filling spout, not shown.

This flexible reservoir-shell 10 is, after filling with the cosmetic product, hermetically sealed by a cover 13 so as to make said reservoir-shell hermetic.

The flexible reservoir shell is either fixed or comprises a head ring 14.

This reservoir-shell of the cosmetic product is subjected to the treatment method according to the invention, the object of which is to destroy with certainty all the microorganisms possibly present in said product and in said reservoir-shell 10.

Once treated, the flexible container-shell 10 is disposed in an over-container 15, forming a rigid peripheral shell capable of carrying the information, communication and any other writing or illustration that would be desirable (Fig.2) .

The ring 14 associated with the reservoir shell fits on the container 15 especially by screwing or clipping (Fig.3).

The reservoir casing 10 is provided with an opening 11 equipped with a screw thread or clipping means for receiving a pump dispenser cap 17, of the "airless" type, that is to say that its operation allows dispensing the product without compensating for the volume of product dispensed by a balanced volume air inlet. The pump-dispenser stopper 17 comprises a cannula 18 for suctioning the product into the reservoir-envelope adapted to perforate the flexible cover 13 during assembly of the head, and to come into contact with the contents of this reservoir shell. flexible (Fig.3).

The over-container has an air inlet 19 because if balancing air is not introduced into the rigid over-container 15, to compensate the delivery of the product. It is necessary to balance the decrease of the volume collapsed by an air inlet in said over-container 15. This air is not in contact with the contents of the reservoir envelope, which poses no problem of re-contamination. The air inlet may be a simple hole possibly provided with a valve or a valve, if it is desired that access to the volume between the envelope and the overcontainer is limited to air only.

The pump-dispenser stopper 17 may be made of a polymer material with biocidal properties or may have been previously treated and taken out of a suitable packaging immediately before it is put in place so as to prevent the introduction of microorganisms. This device is particularly suitable for containing the cosmetic products during the treatment High Hydrostatic Pressures according to the invention, and for the preservation of products once treated.

Advantageously, the combination of the different characteristics of the process according to the invention leads to the irreversible destruction of pathogenic microorganisms that may contaminate the treated cosmetic product.

The microbial agents found in cosmetics are of various types. Various reports or documents specify the nature of these contaminants according to the basic ingredients used, according to the type of cosmetic product and its manufacture, depending on the mode of use (RM BAIRD "Microbial contamination of cosmetics products", J. Soc. Chem (1977), 28, 17-20, R. CAMPANA et al., "Letters in Applied Microbiology (2006)," Microbiological study of cosmetic products for their use by consumers: health risk and efficacy of preservative systems. 43, pp. 301-306, A. VARVARESOU et al., "Self-preserving in cosmetics", Int J Cosmet Sci (2009), 31 (3), p-175, A. DETMER et al. Danish Ministry of Environment Environmental Guideline No. 1336, 2010).

Among these microbial agents contaminating cosmetic products include bacteria (especially those of the Staphylococcus type), molds (like those of the Aspergillus type) and even sometimes spores (this is particularly the case of floral waters or extracts plants used as ingredients in cosmetic compositions).

The method can therefore be used to inactivate at least one pathogenic microorganism in the vegetative state or in the sporulated state present in the cosmetic product.

The invention aims in particular at the use of the method of treating a cosmetic product for the sterilization of cosmetic products and / or to improve their preservation.

The method allows total and irreversible decontamination equivalent to cold sterilization but retaining the internal structure of the cosmetic product and its organoleptic properties.

The specific combination of the parameters of the process according to the invention makes it possible to conduct, in a single step, a total inactivation of the microbial agents contaminating the cosmetic product, whether it be vegetative species or sporulated species. The level can reach depending on the nature of the microorganisms and the composition of the product cosmetic: 10 ⁹ (Destructive Effectiveness ED = 9) for vegetative species, and greater than 10 ⁶ (ED> 6) for sporulated species including bacterial.

According to another aspect, the treatment method according to the invention can also be used to modify the texture of cosmetic products. It is indeed possible to associate with the microbiological safety treatment by application of the method according to the invention, a modification of the texture of the cosmetic product if one introduces during the formulation an ingredient or component (for example a polysaccharide) capable of gelling irreversibly under the conditions of said cosmetic product treatment method according to the invention.

Finally, the invention also relates to a cosmetic product obtained by the implementation of the process, characterized in that it contains no preservative and has an inactivation rate of pathogenic microorganisms present in the medium at least equal to 6 log (destructive efficiency at least equal to 6) relative to the initial product.

By inactivation rate according to the invention, is meant for example:

an inactivation rate of 2 log means that 99% of the pathogenic microorganisms present in the medium are inactivated,

an inactivation rate of 4 log means that 99.99% of the pathogenic microorganisms present in the medium are inactivated,

a rate of 5 log, means that 99.999% of the pathogenic microorganisms present in the medium are inactivated,

a rate of 6 log means that 99.9999% of the pathogenic microorganisms present in the medium are inactivated.

Preferably, the cosmetic product does not contain any preservative and no longer contains any pathogenic microorganism and its properties and structure are identical to those before treatment. As a result, the cosmetic product thus treated by the process retains its natural character. This process seems particularly suitable for products displaying the name "Bio".

In addition, unlike a cosmetic product treated at high temperatures such as thermal pasteurization which eliminates pathogens, the cosmetic product treated according to the invention is not denatured by heat and retains its structure and its properties because the process according to the invention does not heat the cosmetic product at high temperature. Thus, through the process according to the invention, it is possible to obtain cosmetic products without preservatives, bactericides and any additives (intended either to inactivate pathogenic microorganisms or to limit their development) and completely free of microbial contamination without alter the intimate structure of these products and also their organoleptic properties. This treatment is equivalent to cold sterilization.

The conditions of the process according to the invention can be optimized within the ranges of values claimed according to the cosmetic product to be treated, the nature of the pathogenic microorganisms contaminating the product and according to the use sought to obtain the better inactivation rate possible. The conditions can also be optimized within the ranges of values claimed so that the total duration of the treatment process is in agreement with the economic constraints adapted to the treated environment.

The invention is now illustrated by non-limiting examples and tests demonstrating the effectiveness of the method according to the invention.

For these examples, the effectiveness of the process according to the invention with respect to the decontamination of a cosmetic product is evaluated by a number of parameters:

N ₁ represents the initial concentration of microorganisms contaminating the cosmetic product and N _f the final concentration after application of the process according to the invention.

ED is the destructive efficiency related to the process

Example 1

Decontamination test of a cosmetic product without any preservative and untreated by a technique of inactivation of microorganisms.

The effectiveness of the process according to the invention was tested on a cream based on an emulsion and without any addition of preservatives. This cream in addition to water and minority constituents (of the order of 5 to 6%) had a significant concentration in various lipids (vegetable oil, etc.) of more than 15%. It was after its formulation and its preparation placed in a non-sealed container and kept at room temperature for about 4 days.

The initial contamination observed by microbiological analysis was of the order of 3 .10 ⁴ CFU / g. This result highlights, on the one hand, the existence of endogenous contamination initial either derived from the ingredients used in the formulation, or induced by manipulations and secondly that without any preservative this contamination after a few days can reach a significant value, or even significant, because of microbial proliferation.

The various treatment parameters are given in the following Table I as well as the initial contamination (N _i ), the final contamination after HHP treatment (N _f ) and the value of the destructive efficiency (ED) for the endogenous flora.

It is observed that with a cyclic mode of application or a continuous mode (3 cycles of 4min or 12min) the endogenous contamination is totally inactivated at a pressure of 400 MPa and a temperature of 20 ° C or 36 ° C. On the other hand, it was observed that with a cyclic mode of application and at a temperature of 20 ° C. (Test B), the entire microbial load could be inactivated as early as 300 MPa. This result indicates that the process according to the invention makes it possible to inactivate cosmetic products at average pressures and therefore in return to safeguard particularly sensitive assets (or constituents).

It is observed that the application of the process according to the invention under the conditions of Tests B and D leads to a total inactivation of the endogenous flora contaminating the cosmetic product. Example 2

Decontamination tests of the same cosmetic product as that of Example 1 but inoculating doses of various microorganisms.

To evaluate the destructive efficiency of the process according to the invention, two microorganisms were selected for the test challenges: a Gram + bacterium (Staphylococcus aureus) and a mold (Aspergillus brasiliensis) often considered by the community of people in the sector. cosmetics as contaminants often encountered.

The same values of the process parameters according to the invention were applied as those mentioned in Example 1 (Tests A to D) (see Table I).

From the application of these representative tests of the process according to the invention, it can be concluded:

(i) Under the same conditions of treatment Aspergillus brasiliensis seems more sensitive to the application of the process than Staphylococcus aureus

(ii) To completely inactivate Staphylococcus aureus under the conditions of this study, it is necessary to have a cyclic application (here 3 cycles of 4 min and a pressure of 400 MPa either at 20 ° C or at 36 ° C C) (see Tests B and D)

(iii) It is interesting to point out that it is possible to reach for this bacterium

Gram + reputed to be very baroresistant in the prior art, ED values of the order of 7. Example 3

Test of the process according to the invention for the sterilization of cosmetic products on another cream having characteristics very different from those tested in Examples 1 and 2.

The cosmetic product tested differs from the previous one by the fact that no initial contamination (before any voluntary inoculation of microorganisms) was observed.

The following table (Table III) gives the treatment parameters according to the processes according to the invention which have been used.

This product has been inoculated with doses of micro-organisms (challenges-tests). Two types of microorganisms were used: a Gram + bacterium (Staphylococcus aureus) and a mold (Aspergillus brasiliensis) considered by the community of people in the cosmetic sector as contaminants often encountered.

The efficiency of destruction of these microorganisms after application of the method according to the invention of decontamination of cosmetics products (with the process parameters mentioned in Table III) is given in Table IV.

It is also noted, as for the preceding product (see Example 2), that the mold-type microorganism (Aspergillus brasiliensis) is more sensitive to the effects of the process according to the invention than the Gram + Staphylococcus aureus bacterium, since, whatever the conditions, the inactivation is total.

On the other hand, the conditions for the total inactivation of Staphylococcus aureus are more drastic but they appear identical to those observed for the other cosmetic product (see Example 2).

It thus appears possible through the selection of the process parameters according to the invention to be able to inactivate completely and irreversibly all of the microbial load (Aspergillus brasiliensis and Staphylococcus aureus). This total and irreversible inactivation is similar to cold sterilization.

Example 4

The total decontamination of a cosmetic product by the process according to the invention could be applied industrially only if the intimate structure of the product remained unaltered after application of such an HHP process.

Representative images of the cosmetic products have been observed a set of small bubbles characteristic of an emulsion of uniform size covering the entire surface under the microscope.

After treatment according to conditions leading to total inactivation of inoculated pathogenic microorganisms (Aspergillus brasiliensis and Staphylococcus aureus) microscopic observation (magnification x500) shows uniform size bubbles covering the entire surface of the microscope stage with a distribution identical to the control sample. It follows that the intimate structure of the cream (emulsion) has not been altered by the treatment according to the method of high hydrostatic pressures. The organoleptic properties (color, smell and visual appearance) are also saved.

The implementation of the method according to the invention therefore leads to a total inactivation of contaminating microorganisms, without altering the intimate structure of the product or its organoleptic properties (color, odor and visual appearance).

Example 5

A cosmetic cream without any preservative or additive capable of inducing a bactericidal effect or limiting the growth of microorganisms has been deliberately contaminated (challenges-tests) by 4 microbial species or in the vegetative state [Staphylococcus aureus ATCC 6538, Enterobacter aerogeneses ATCC 13048) or sporulated (Aspergillus brasiliensis ATCC 16404).

The cream thus contaminated was subjected to 2 HHP treatments according to the invention (see Table VII).

The results obtained are shown in Table VII below.

Example 6

The same cosmetic cream as in Example 5, without any preservative or additive likely to induce a bactericidal effect or to limit the growth of microorganisms, was voluntarily contaminated (challenges-tests) by 2 microbial species either at the same time. vegetative state (Staphylococcus aureus ATCC 6538), or in the sporulated state [Bacillus cereus ATCC14579).

The conditions of the HHP treatments of this cream are given in Table VIII.

The results of the microbiological analyzes are given in Table IX.

Example 7

The same cosmetic cream as that used for Examples 5 and 6, therefore without any preservative or bactericidal additive, was inoculated on the one hand by the vegetative Staphylococcus aureus species with a very high initial level of contamination, close to 10 ⁹ CFUs. / mL, and secondly by a sporulated species Bacillus cereus with an initial level of contamination close to 10 ⁶ CFU / mL.

This cream has been placed in a flexible and deformable container in order to be certain to transmit the parameters characteristic of the Hydrostatic High Pressure Process (HHP) to the product. This test container is then sealed to prevent recontamination of the cream by the pressure transmitter medium.

The characteristic parameters of the HHP treatment process are given in Table X.

The duration of application of the pressure for each cycle is 5 minutes At the end of this treatment, the untreated control and the treated cream sample are used for sowing in the media suitable for the growth of these microorganisms. After incubation counts are then made. The results of these microbiological analyzes are given in Table XI.

Claims

1. A method for treating a cosmetic product by high hydrostatic pressure, consisting in applying to the cosmetic product a pressure P of between 200 MPa and 600 MPa with a continuous or cyclic MA application mode, with a speed VA of application of the pressure P for the compression between 0.5 and 50 MPa / s.

2. Process for treating a cosmetic product according to one of the preceding claims, characterized in that speed decompression rate of between 1 and 50 MPa / s.

3. Process for treating a cosmetic product according to claim 1, characterized in that the total duration t of application of the pressure P of between 2 and 60 minutes.

4. Process for treating a cosmetic product according to one of the preceding claims, characterized in that the initial temperature Ti of the cosmetic product to be treated between -10 ° C and 40 ° C.

5. Process for treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that the duration of application of the pressure P of each cycle is between 2 and 20 minutes.

6. Process for treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that at least two cycles have a duration applying different pressure P.

7. Process for treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that for at least two of the cycles the pressure P to the cosmetic product is different.

8. Process for treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that the pressure between two cycles is:

o the ambient pressure or

o an intermediate pressure between ambient pressure and the most high pressures P applied during said two cycles.

9. A method of treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that at least two of the cycles have a compression speed VA and / or different decompression.

10. A method of treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that for at least one cycle the compression speed VA and / or the speed of decompression varies until reaching the pressure P.

11. Process for treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that at least two cycles have a different compression and / or decompression profile. .

12. Process for treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that for the same cycle, the compression profile and the decompression profile are different. .

13. A method of treating a cosmetic product according to one of the preceding claims, characterized in that the application mode MA is cyclic and in that between at least two cycles, there is a latency

14. Process for treating a cosmetic product according to claim 14, characterized in that it comprises at least three cycles and at least two latency times. different.

15. Process for treating a cosmetic product according to claim 14 or 15, characterized in that the latency time is between 2 and 20 minutes.

16. A method of treating a cosmetic product according to one of the preceding claims, characterized in that it is implemented in a high pressure chamber closed by at least one shutter.

17. A method of treating a cosmetic product according to one of the preceding claims, characterized in that the cosmetic product is packaged in its final packaging or in part of its final packaging for the implementation of the method.

18. A method of treating a cosmetic product according to one of the preceding claims, characterized in that the cosmetic product is a cosmetic composition intended to be applied to the skin, mucous membranes or integuments.

19. Process for treating a cosmetic product according to one of claims 1 to 18, characterized in that the cosmetic product is a cosmetic active ingredient or a cosmetic excipient intended to be integrated into a cosmetic composition.

20. Use of the method of treating a cosmetic product according to one of claims 1 to 20, for inactivating in a single step of treatment at least one pathogenic microorganism in the vegetative state or the sporulated state present in the product. cosmetic.

21. Use of the method of treating a cosmetic product according to one of claims 1 to 20, for the sterilization of cosmetic products.

22. Use of the method of treating a cosmetic product according to one of claims 1 to 20, for improving the preservation of cosmetic products.

23. Use of the method of treating a cosmetic product according to one of claims 1 to 20, for modifying the texture of cosmetic products by introducing during the formulation of these products prior to their treatment a constituent capable of irreversibly geling under the conditions of said cosmetic product treatment method.

24. Cosmetic product obtained by the implementation of the method according to one of claims 1 to 20, characterized in that it contains no preservative or bactericidal agent and in that it has an inactivation rate pathogenic microorganisms present in the product at least equal to 6 log (destructive efficiency at least equal to 6) relative to the initial product but may according to the combination of the process parameters, adapted to the nature of the contaminating microorganisms and to product composition, reach 9 log.

25. Cosmetic product obtained by the implementation of the method according to one of claims 1 to 20, characterized in that its properties and structure are identical to those before treatment, it does not contain preservative or bactericidal, that it contains no pathogenic micro-organism.

26. Device adapted for implementing the method according to one of claims 1 to 19, characterized in that it comprises a container (10) flexible, closed, for receiving a product (12), the entire container and the product having been treated by the method according to one of claims 1 to 19, an over-container (15) for receiving said flexible container with its product (12), after treatment, a stopper dispenser (17) provided with a suction cannula (18) adapted to perforate the lid (13) of said flexible envelope.

27. Device according to claim 26, characterized in that the over-container (15) comprises an air inlet (19).

28. Device according to claim 26 or 27, characterized in that the casing is a flexible envelope comprising an opening (11) in the upper part, a cap (13) to make said reservoir-shell hermetic and a head ring (14). ) intended to cooperate with the over-container (15).