CN111374899B - Composition and preparation method and application thereof - Google Patents
Composition and preparation method and application thereof Download PDFInfo
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- CN111374899B CN111374899B CN201911396572.5A CN201911396572A CN111374899B CN 111374899 B CN111374899 B CN 111374899B CN 201911396572 A CN201911396572 A CN 201911396572A CN 111374899 B CN111374899 B CN 111374899B
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/35—Ketones, e.g. benzophenone
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K8/00—Cosmetics or similar toiletry preparations
- A61K8/18—Cosmetics or similar toiletry preparations characterised by the composition
- A61K8/30—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds
- A61K8/33—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing oxygen
- A61K8/34—Alcohols
- A61K8/345—Alcohols containing more than one hydroxy group
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K2800/00—Properties of cosmetic compositions or active ingredients thereof or formulation aids used therein and process related aspects
- A61K2800/40—Chemical, physico-chemical or functional or structural properties of particular ingredients
- A61K2800/52—Stabilizers
- A61K2800/524—Preservatives
Abstract
The invention discloses a composition, a preparation method and application thereof. The composition comprises the following components in percentage by mass: 15-30% of p-hydroxyacetophenone, 1-10% of caprylic glycol and/or caprylic glyceride, 5-55% of hexanediol and/or isoprene glycol, and the balance is made up to 100% by using dipropylene glycol. The composition of the invention is safe, mild and non-irritant when used as a compound preservative; the pH and temperature application range is wide, and the stability is good; the appearance is liquid, the water solubility is good, the use is convenient, and the preservative effect is excellent.
Description
Technical Field
The invention belongs to the field of cosmetics, and particularly relates to a composition, and a preparation method and application thereof.
Background
The cosmetic preservative means a substance added to the cosmetic for the purpose of inhibiting the growth and reproduction of microorganisms in the cosmetic. During the production and use of cosmetics, it is inevitable to mix some microorganisms, which are one of the important causes of spoilage of cosmetics. The preservative in the cosmetic mainly has the effects of inhibiting the growth and reproduction of microorganisms, keeping the stable property of the cosmetic, preventing the cosmetic from deteriorating after being uncapped for use and providing the required preservative effect of the cosmetic during storage and use.
The preservative used in the cosmetics is traditionally prepared by adopting cosmetic regulations to solve the problem of corrosion prevention of the cosmetics by using one or more of 51 preservatives in a compounding way. The traditional preservative is a limited substance, and is used for solving the problem of corrosion prevention of cosmetics by only using a certain preservative, so that the corrosion prevention effect is difficult to ensure, the dosage needs to be increased, and the problem of product safety can be caused by increasing the dosage, so that more than 2 preservatives are generally used in the cosmetics.
Traditional preservatives suffer from more or less of these problems, with some negative reports of less and less tendency to be used in cosmetics. Conventional preservatives commonly used in cosmetics include parabens, phenoxyethanol, formaldehyde-releasing agents (imidazolidinyl urea, etc.), MIT (methylisothiazolinone), etc. Parabens report a potential risk of causing breast cancer; the formaldehyde slow-release body preservative mainly slowly releases a very small amount of free formaldehyde in a cosmetic system, so that the very high-efficiency effect of the formaldehyde in killing microorganisms is exerted, the cosmetics are prevented from being damaged by the microorganisms, the free formaldehyde is a recognized substance harmful to human bodies and the environment and is one of the reasons for causing biological variation, the formaldehyde releaser is not high-temperature resistant, and the preservative effect can be ensured only by adding the formaldehyde releaser at the temperature lower than 40 ℃ when in use; MIT reported to cause skin allergy and has been banned from use in leave-on cosmetics in the european union; higher amounts of phenoxyethanol also cause skin stinging or burning. With the rising concern of people on self safety and health and the continuous enhancement of environmental protection concepts, more and more people begin to worry about the safety problem of the traditional preservative. This concern is continually increasing with the continued publicity of media and public opinion. The reduction or even elimination of traditional preservatives has been a public opinion hotspot and trend.
Along with the development of economy and the improvement of living standard of people, the frequency of using cosmetics is higher and higher, people know more and more about the cosmetics, and the requirements on the safety and the quality of the cosmetics are higher and higher.
Good preservatives not only need to prevent and inhibit the growth of microorganisms such as bacteria and fungi, but also must be safe, mild, non-irritating to the human body, non-reactive with other chemical components of the formulation, stable at different PHs and temperatures, and provide the desired preservative function during storage and use of the cosmetic.
Although there are patents related to non-traditional preservatives in the prior art (e.g., CN 107624758A, etc.), most complex preservatives require additional solubilizing agents. For example: in patent application CN 107624758A, hydroxyacetophenone is dissolved using a mixture of one or more of solvents 1, 2-propylene glycol, 1, 3-propylene glycol, polyethylene glycol 400, however, the solubility of this mixture is not high and needs to be dissolved upon heating, and once returned to room temperature, hydroxyacetophenone precipitates out and precipitates out more rapidly upon refrigeration or cooling to-18 ℃. The content difference of the upper and lower layers of p-hydroxyacetophenone in the antiseptic composition is large, and the components are not uniform, so that the proportion of the antiseptic in the antiseptic composition added into a product is not uniform, the antiseptic effect of the antiseptic composition is seriously influenced, and the antiseptic composition is inconvenient to use. Thus, in this patent application, solubilizing agents alkylphenol ethoxylates, fatty alcohol polyoxyethylene ethers, and hydrogenated castor oil polyoxyethylene ethers, all of which contain polyoxyethylene ethers, are also selected to increase the low-temperature solubility of p-hydroxyacetophenone. The ingredients containing polyoxyethylene ether contain more or less Dioxane ingredients according to different production processes, the Dioxane (1, 4-Dioxane) is a byproduct for producing compounds containing polyoxyethylene ethers, the Dioxane (1, 4-Dioxane) can be carcinogenic and is listed as a carcinogenic substance, the IARC is divided into 2B, the Dioxane belongs to components which are prohibited to be added as production raw materials in cosmetics, products containing the ingredients have certain potential risks, the insecurity of the substances prepared by using the Dioxane can be increased, and the products are not popular with consumers.
Disclosure of Invention
The invention aims to solve the technical problem of providing a composition, a preparation method and application thereof in order to overcome the defects of low solubility or carcinogenic risk of a solubilizer for dissolving p-hydroxyacetophenone in the existing compound preservative. The composition of the invention is safe and mild and has no stimulation when being used as a compound preservative; the pH and temperature application range is wide, and the stability is good; the appearance is liquid, the water solubility is good, the use is convenient, and the anti-corrosion effect is excellent.
The inventor creatively adopts the cosmetic rules (technical Specification for cosmetic safety) to allow the use of 51 preservatives (such as parabens, phenoxyethanol, imidazolidinyl urea, diazolidinyl urea, 1, 3-dimethylol-5, 5-dimethylhydantoin, chlorphenesin and the like) and other cosmetics, such as pentanediol, hexanediol, octaglycol, glycerol caprylate and/or p-hydroxyacetophenone and the like as preservatives, to be compounded in a certain proportion to obtain the composition of the invention, thereby exerting the advantages of each raw material, and ensuring the use stability and the preservative effect of the composition while reducing the use amount of the preservative raw material as much as possible. If the single use of the caprylyl glycol, the caprylic glyceride, the hexanediol or the p-hydroxyacetophenone is used as the preservative, the addition amount of the caprylyl glycol, the caprylic glyceride or the hexanediol needs to be increased remarkably in order to meet the preservative requirement of the cosmetics, and although the substances are non-limiting substances and are not limited in use, the three substances, namely the caprylyl glycol, the caprylic glyceride and the hexanediol have certain surface activity and certain permeability; meanwhile, the larger the using amount is, the larger the amount penetrating the skin is, when the amount penetrating the skin is large to a certain degree, the more the amount exceeds the tolerance concentration of a human body, the potential irritation is caused, and when the amount penetrating the skin is large to a certain degree, the more the phenol hydroxyl group exists in the structure, the water solubility is good, the higher the concentration is, the stronger the effect of the phenol hydroxyl group is, the larger the irritation is), the skin thermal sensation and the skin irritation are obviously increased (the individual difference of people is different, the concentrations of the thermal sensation and the irritation are different, when the capryl glycol, the capryl glyceride, the hexanediol and the p-hydroxyacetophenone are tested by consumers in a laboratory, the irritation is caused to the skin when the concentration exceeds a certain concentration, and the irritation is also a common consensus of the cosmetic industry. The safety and the mildness of the product can not meet the requirements at all. The inventor combines the raw materials organically after creative work, and the raw materials are synergistic, so that the use amounts of the caprylic glycol, the caprylic glyceride, the hexanediol and the p-hydroxyacetophenone can be reduced effectively, the safety of the preservative is improved greatly, and meanwhile, the preservative challenge meets the preservative requirement of cosmetics; and no additional solubilizer is required.
The invention solves the technical problems through the following technical scheme.
The invention provides a composition, which comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of caprylic glycol and/or caprylic glyceride, and 5 to 55 percent of hexanediol and/or isoprene glycol, and the dipropylene glycol is used for complementing to 100 percent.
Preferably, the mass percent of the hexanediol and/or the isoprene glycol in the composition is 11-15%, for example, the mass percent of the hexanediol is 10%, and the mass percent of the isoprene glycol is 5% or 1%.
In the present invention, the composition preferably comprises the following components in percentage by mass: 15-30% of p-hydroxyacetophenone, 1-10% of caprylic glycol and/or caprylic glyceride, 5% of isoprene glycol and dipropylene glycol;
alternatively, the composition preferably comprises the following components in percentage by mass: 15-30% of p-hydroxyacetophenone, 1-10% of caprylic glycol and/or caprylic glyceride, 10-50% of hexanediol and dipropylene glycol;
or the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of caprylic glycol and/or caprylic glyceride, 1 to 5 percent of isoprene glycol, 10 to 50 percent of hexanediol and dipropylene glycol.
Wherein, the mass percentage of the p-hydroxyacetophenone is preferably 15 to 22 percent or 22 to 30 percent, and more preferably 22 percent.
The mass percentage of the caprylic glycol and/or the caprylic glycol ester is preferably 1 to 6 percent or 6 to 10 percent, and more preferably 6 percent.
The hexanediol is preferably present in an amount of 5% to 30% by weight, or 30% to 50% by weight, more preferably 30% by weight.
In the present invention, in order to enhance the moisturizing effect of the composition and skin feel adjustment when the composition is applied to a skin care product, and simultaneously promote or assist the dissolution of p-hydroxyacetophenone in the composition, and enhance the preservative effect, the composition further comprises an auxiliary component comprising one or more of pentanediol, 1, 3-butanediol, and 1, 3-propanediol. Preferably, the content of the auxiliary component is 1-10%, and the percentage is the mass percentage of the composition.
In a preferred embodiment of the present invention, the composition comprises the following components: 22% p-hydroxyacetophenone, 6% caprylic glycol or caprylic glyceride and 30% hexylene glycol, with dipropylene glycol to make up to 100%.
In another preferred embodiment of the present invention, the composition comprises the following components: 30% of p-hydroxyacetophenone, 1% of octaethylene glycol, 10% of hexanediol and 1% of isoprene glycol, with dipropylene glycol to make up to 100%.
In another preferred embodiment of the present invention, the composition comprises the following components: 15% of p-hydroxyacetophenone, 10% of glyceryl caprylate and 50% of hexylene glycol, the balance being dipropylene glycol to 100%.
In another preferred embodiment of the present invention, the composition comprises the following components: 30% of p-hydroxyacetophenone, 1% of glyceryl caprylate and 10% of hexanediol, with dipropylene glycol to make up to 100%.
In another preferred embodiment of the present invention, the composition comprises the following components: 15% p-hydroxyacetophenone, 10% octyl glycol and 50% hexylene glycol, with dipropylene glycol to make up to 100%.
In another preferred embodiment of the present invention, the composition comprises the following components: 30% of p-hydroxyacetophenone, 1% of octanediol and 10% of hexanediol, with dipropylene glycol making up to 100%.
In another preferred embodiment of the present invention, the composition comprises the following components: 30% of p-hydroxyacetophenone, 10% of glyceryl caprylate and 5% of isoprene glycol, with dipropylene glycol to make up to 100%.
In another preferred embodiment of the present invention, the composition comprises the following components: 30% of p-hydroxyacetophenone, 10% of octanediol and 5% of isoprene glycol, the balance being dipropylene glycol to 100%.
In another preferred embodiment of the present invention, 15% p-hydroxyacetophenone, 10% glyceryl caprylate, 50% hexylene glycol and 5% isoprene glycol are supplemented with dipropylene glycol to make up to 100%.
In another preferred embodiment of the present invention, 30% p-hydroxyacetophenone, 1% glyceryl caprylate, 10% hexylene glycol and 5% isoprene glycol are supplemented with dipropylene glycol to make up to 100%.
In another preferred embodiment of the present invention, 15% of p-hydroxyacetophenone, 10% of octanediol, 50% of hexanediol and 5% of isoprene glycol are supplemented with dipropylene glycol to 100%.
In another preferred embodiment of the present invention, 30% p-hydroxyacetophenone, 1% octylene glycol, 10% hexylene glycol and 5% isoprene glycol are supplemented with dipropylene glycol to make up 100%.
In another preferred embodiment of the present invention, the composition consists of: 30% of p-hydroxyacetophenone, 10% of glyceryl caprylate, 5% of isoprene glycol and 55% of dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 30% of p-hydroxyacetophenone, 10% of octanediol, 5% of isoprene glycol and 55% of dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 22% of p-hydroxyacetophenone, 6% of caprylic glycol and/or caprylic glyceride, 30% of hexylene glycol, and 42% of dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 30% p-hydroxyacetophenone, 1% octanediol, 10% hexanediol, 1% isoprene glycol, and 58% dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 15% p-hydroxyacetophenone, 10% glyceryl caprylate, 50% hexylene glycol, and 25% dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 30% of p-hydroxyacetophenone, 1% of glyceryl caprylate, 10% of hexylene glycol, and 59% of dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 15% of p-hydroxyacetophenone, 10% of octanediol, 50% of hexanediol, and 25% of dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 30% of p-hydroxyacetophenone, 1% of octaethylene glycol, 10% of hexanediol, and 59% of dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 15% p-hydroxyacetophenone, 10% glyceryl caprylate, 50% hexylene glycol, 5% isoprene glycol, and 20% dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 30% p-hydroxyacetophenone, 1% glyceryl caprylate, 10% hexylene glycol, 5% isoprene glycol, and 54% dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 15% of p-hydroxyacetophenone, 10% of octanediol, 50% of hexanediol, 5% of isoprene glycol, and 20% of dipropylene glycol.
In another preferred embodiment of the present invention, the composition consists of: 30% of p-hydroxyacetophenone, 1% of octanediol, 10% of hexanediol, 5% of isoprene glycol, and 54% of dipropylene glycol.
The above percentages are mass percentages.
The invention also provides a preparation method of the composition, which comprises the steps of mixing the mixture of the dipropylene glycol, the hexanediol and the caprylic glycol and/or the caprylic glyceride with the p-hydroxyacetophenone, and heating for dissolving to obtain the composition;
wherein the degree of heating (e.g., time, temperature, etc.) is preferably such that the p-hydroxyacetophenone is dissolved without destroying the activity of the components of the composition, as is well known in the art.
Preferably, the preparation method comprises the following steps:
(1) Heating a mixture of the dipropylene glycol, the hexylene glycol and/or isoprene glycol, and the caprylic glycol and/or the caprylic glyceride to dissolve;
(2) Adding the p-hydroxyacetophenone, heating for dissolving, and cooling.
In the step (2), the state after dissolving by heating may be conventional in the art, and is preferably a transparent state.
In step (2), the temperature after cooling may be conventional in the art, such as room temperature; the room temperature is room temperature in the usual sense, preferably 15 to 25 ℃.
The invention also provides an application of the composition as a composite preservative in skin care products or cosmetics.
Preferably, the composition acts as a compound preservative to inhibit the growth of one or more of bacteria, mold and yeast; wherein:
the bacteria are preferably selected from one or more of Escherichia coli (Escherichia coli), pseudomonas cepacia (Pseudomonas cepacia), pseudomonas aeruginosa (Pseudomonas aeruginosa) and Staphylococcus aureus (Staphylococcus aureus);
the mould is preferably Aspergillus niger;
the yeast is preferably Candida albicans (Candida albicans).
Preferably, the concentration of the composition in the skin care product or the cosmetic product is 0.5% to 2%, such as 1.4%, 1.7%, or 1.5%, said percentages being percentages by mass.
On the basis of the common knowledge in the field, the above preferred conditions can be combined randomly to obtain the preferred embodiments of the invention.
The reagents and starting materials used in the present invention are commercially available.
The positive progress effects of the invention are as follows:
the composition is safe, mild and non-irritant when being used as a compound preservative; the pH and temperature range of use is wide, for example: the application range of the pH can be 5-9 (the maximum applicable pH can reach 9 and the minimum can reach 5), the temperature range can be-18-45 ℃, and the stability is good; the appearance is liquid, the water solubility is good, the use is convenient, and the anti-corrosion effect is excellent.
Drawings
FIG. 1 shows the different solutions after standing for one month at 4 ℃.
Detailed Description
The invention is further illustrated by the following examples, which are not intended to limit the scope of the invention. The experimental methods without specifying specific conditions in the following examples were selected according to the conventional methods and conditions, or according to the commercial instructions.
In the following examples, "%" is defined as mass% unless otherwise specified.
Escherichia coli, pseudomonas cepacia, pseudomonas aeruginosa, staphylococcus aureus, aspergillus niger, and Candida albicans were purchased from ATCC (American type culture Collection).
Tryptone soy broth, yeast malt extract medium, and Letheen broth were purchased from shanghai guanwei instruments ltd; lecithin tween medium and bengal red medium were purchased from shanghai starter co.
The compositions are used as compound preservatives in the following examples.
The compound preservatives used in the following examples were prepared by the following methods:
(1) Heating and dissolving a mixture of dipropylene glycol, hexylene glycol (and/or isoprene glycol), and caprylic glycol (or caprylic glyceride);
(2) Adding p-hydroxyacetophenone, heating to dissolve, and cooling to room temperature.
The degree of heating (e.g., time, temperature, etc.) is preferably such that the hydroxyacetophenone is dissolved without destroying the activity of the components of the composition, as is conventional in the art.
EXAMPLE 1 effectiveness of preservatives of different ratios
Preservative efficacy at different preservative combinations was verified by preservative challenge tests.
TABLE 1 Experimental samples
The formula proportion information of the basic skin lotion A/B/C/D/E/F/N/O is as follows:
0.05% of EDTA disodium; 0.10% allantoin; 0.20% Tremella (Tremella FUCIFORMIS) extract; 4.00% glycerol; 1.00% sorbitol; 1.00 percent of wall-broken yeast extract; compound preservative (the specific formula and dosage are shown in the table); adjusting the pH value to 7 by proper amount of citric acid and potassium hydroxide, and adding water to the rest (the percentages are mass percentages).
Experimental strains
Escherichia coli (Escherichia coli), pseudomonas cepacia (Pseudomonas cepacia), pseudomonas aeruginosa (Pseudomonas aeruginosa), staphylococcus Aureus (Staphylococcus Aureus), aspergillus niger (Aspergillus niger), and Candida albicans (Candida albicans).
Experimental reagent
Tryptone soy broth, yeast malt extract medium, letheen broth, lecithin tween medium, and Bengal red medium.
Pretreatment of the experiment
The addition concentration of the bacteria (Escherichia coli, pseudomonas cepacia, pseudomonas aeruginosa and Staphylococcus aureus) was 10 8 The addition concentration of mould (Aspergillus niger) and yeast (Candida albicans) is 10% 7 And/ml. The experimental recording time points were day 2, 7, 14, 21, 28 respectively after the start of the experiment, with repeated challenges on day 21.
Inoculation method (preservation challenge experiments in the following examples are all the same inoculation method)
1. Adding 5ml tryptone soybean broth culture medium into a shake tube, scraping an inoculating loop of lawn from the slant culture medium, and inoculating into tryptone soybean broth, wherein the total amount of 5 mycelia (including four bacteria and a blank) are obtained; adding 7ml of yeast malt extract culture medium into a shake tube, adding 2 yeast malt extract culture medium (the concentration of yeast is low, 2 yeast strains need to be inoculated), adding 5ml of yeast malt extract culture medium into a blank shake tube, scraping one inoculation ring of lawn from the slant culture medium, and inoculating into 7ml of yeast malt extract culture medium. Culturing bacteria in a gas bath at 32 deg.C and 150rpm for 20 hr, culturing yeast for 22 hr, and taking out.
2. Preparing a 96-well plate in advance, adding 200ml of the bacterial liquid into the wells of the 96-well plate, adding each bacterial liquid twice, adding a blank culture solution, placing the blank culture solution into an enzyme-labeling instrument to measure the OD value of the blank culture solution, multiplying the obtained OD value by the constant of the strain to obtain the actual bacterial liquid concentration, adjusting the dilution or concentration multiple according to the calculated concentration, and adjusting the actual bacterial addition concentration to be 10 8 Per ml, fermentingThe actual concentration of the mother bacteria is 10 7 /ml。
3. Absorbing 1ml of each of the four bacteria with the concentration to prepare a comprehensive bacterial liquid for later use.
4. And (3) sucking 1ml of the comprehensive bacterium liquid, adding the comprehensive bacterium liquid into 100g of a sample (the sample is the basic skin moisturizer to be tested, and if no special explanation is given, the explanation is applicable), stirring the mixture to be as uniform as possible by using a sterile stirring rod, and culturing the mixture in an incubator with 25 ℃ and 60% humidity. Sucking 1ml of sample with a needle tube on the 2 nd day (abbreviated as "D"), 7 th day, 14 th day, 21 th day and 28 th day after the culture, adding into a small bottle containing 9ml of leteen broth, shaking up, taking 1ml of the mixed solution, adding into a clean plate, pouring lecithin Tween 80 medium, sucking 1ml of the mixed solution, adding into the next small bottle containing 9ml of leteen broth, repeating twice, namely, diluting in a total gradient of 10 4 And (4) doubling. This operation was repeated for each sample.
5. Each flask of medium used required a blank plate to control for contamination of the medium.
6. And repeating the operations 2, 3 and 8 on the 21 st day, and adding the bacterial or fungal mixed bacteria liquid into the sample, namely repeating the challenge.
7. The completely coagulated medium was inverted, placed in a 37 ℃ incubator for 2 days, and observed and read.
8. The yeast strain having reached the concentration mentioned in the point 2 was aspirated by 1ml into an empty bottle, and 1ml of the spore suspension prepared in advance was aspirated to prepare a mixed fungal solution for use.
9. The mixed fungal solution was aspirated at 1ml and added to 100ml of sample, and the procedure in point 4 was repeated, but Bengal red medium was poured into the plate and a blank plate reference was set.
10. The completely coagulated Bengal culture medium was inverted, placed in a 28 ℃ incubator for 3 days, and observed and read.
11. Reading: the plate is placed upside down under a magnifying glass, the number of colonies on the plate is counted, and the concentration of the colonies in the sample at the moment is calculated.
Results of the experiment
TABLE 2
Conclusion of the experiment
As can be seen from tables 1 and 2, all samples pass the corrosion protection challenge test, which shows that the compound preservative can achieve effective corrosion protection under different mixture ratio combinations within the application range.
Example 2 sensitization study of a Compound preservative-aqueous Patch test
The composite preservative is diluted into 1.5 percent (mass percentage) of aqueous solution, and the sensitization of the aqueous solution is verified by a patch test. The results of the verification show that the complex preservative of the present invention exhibits absolute mildness (0 cases of sensitization phenomenon) even at high addition levels.
The patch sensitization study is reported in detail below:
inspection Unit
Shanghai city skin disease hospitals.
Test acceptance number
PT-I-2018-0140。
Basis of examination
Technical Specifications for cosmetic safety (2015 edition).
Materials and methods
1. The test substance: the compound preservative is 1.5% aqueous solution (the formula of the compound preservative is 58% dipropylene glycol, 30% p-hydroxyacetophenone, 10% hexanediol, 1% octylene glycol and 1% isoprene glycol, and the percentages are mass percentages).
2. Negative control: and (6) filtering the paper.
3. Subject: the total number of 30 persons, 8 men and 22 women, the age of 21-60 years, meets the volunteer selection standard of the subject.
4. The spot test method comprises the following steps: selecting a qualified spot tester, placing 0.020-0.025 mL of a tested object in the spot tester by a closed spot test method, externally applying a special adhesive tape to the back of the tested object, removing the tested object after 24 hours, observing skin reactions respectively at 0.5, 24 and 48 hours after removal, and recording the results according to the skin reaction grading standard in technical Specification for cosmetic safety (2015 edition).
Test results
As can be seen from table 3, the composition of the present invention is safe, mild and non-irritating when used as a compound preservative.
TABLE 3 cosmetic human skin Patch test results
Example 3 sensitization study of a Compound preservative-facial mask fluid Patch test
In order to better simulate the sensitization research of the compound preservative applied to the skin care products, the compound preservative is added into a typical facial mask liquid formula, the addition amount is 1.0 percent (the addition amount in the recommended facial mask liquid formula), and the sensitization is verified by a patch test. The results of the verification showed that the complex preservative of the present invention exhibited absolute mildness (0 sensitization) even at the highest addition level.
Formula information: 0.05% of EDTA disodium, 0.10% of allantoin, 0.03% of tremella extract, 8.00% of glycerin, 2.00% of betaine, 0.18% of carbomer 914, 0.18% of triethanolamine, 0.50% of wall-broken yeast extract, 0.50% of dendrobium officinale extract and 1.00% of compound preservative; and 75.46% deionized water.
The patch sensitization study is reported in detail below:
inspection unit
Shanghai city skin disease hospital.
Test acceptance number
PT-I-2018-0105。
Basis of examination
Technical Specifications for cosmetic safety (2015 edition).
Materials and methods
1. The test substance: the moisture facial mask contains 1% of compound antiseptic (the formula of the compound antiseptic is 58% dipropylene glycol, 30% p-hydroxyacetophenone, 10% hexanediol, 1% octanediol and 1% isoprene glycol)
2. Negative control: blank control.
3. Subject: the total number of 30 persons, 10 men and 20 women, the age is 28-59 years, and the volunteer enrollment criteria of the subject are met.
4. The spot test method comprises the following steps: selecting a qualified spot tester, placing 0.020-0.025 mL of a tested object in the spot tester by a closed spot test method, externally applying a special adhesive tape to the back of the tested object, removing the tested object after 24 hours, observing skin reactions respectively at 0.5, 24 and 48 hours after removal, and recording the results according to the skin reaction grading standard in technical Specification for cosmetic safety (2015 edition).
Test results
As can be seen from table 4, the composition of the present invention is safe, mild and non-irritating when used as a complex preservative.
TABLE 4 cosmetic human skin Patch test results
EXAMPLE 4 Corrosion efficacy Studies of a Compound preservative at different pHs
And randomly selecting a preservative combination, and verifying the preservative efficacy of the compound preservative through a preservative challenge test in different formula pH environments.
TABLE 5 test samples
The formula proportion information of the basic skin care lotion G/H/I/J/Q/R is as follows:
0.05% of EDTA disodium; 0.10% allantoin; 0.20% Tremella (Tremella FUCIFORMIS) extract; 4.00% glycerol; 1.00% sorbitol; 1.00 percent of wall-broken yeast extract; compound preservative (the specific formula and dosage are shown in the table); proper amount of citric acid and potassium hydroxide is used for adjusting the pH value to the current value (5.0/7.0/9.0), and the rest is water.
Experimental strain
Escherichia coli (Escherichia coli), pseudomonas cepacia (Pseudomonas cepacia), pseudomonas aeruginosa (Pseudomonas aeruginosa), staphylococcus Aureus (Staphylococcus Aureus), aspergillus niger (Aspergillus niger), and Candida albicans (Candida albicans).
Experimental reagent
Tryptone soy broth, yeast malt extract medium, letheen broth, lecithin tween medium, and Bengal red medium.
Pretreatment of the experiment
The bacteria (Escherichia coli, pseudomonas cepacia, pseudomonas aeruginosa and Staphylococcus aureus) were added at a concentration of 10 8 The addition concentration of mould (Aspergillus niger) and yeast (Candida albicans) is 10 7 . The experimental recording time points were day 2, 7, 14, 21, 28 respectively after the start of the experiment, with repeated challenges on day 21.
TABLE 6 results of the experiment
Conclusion of the experiment
As can be seen from tables 5 and 6, all samples passed the preservative challenge test, demonstrating that the compound preservative is effective in preserving at different pH environments.
EXAMPLE 5 Corrosion efficacy Studies of a composite preservative at different temperatures
Randomly selecting an antiseptic combination; the preservative effectiveness of the compound preservative is verified by a preservative challenge test under production processes with different addition temperatures.
TABLE 7 test samples
Formula proportioning information of the basic skin lotion:
phase I: 0.05% edta disodium; 0.10% allantoin; 0.20% Tremella (Tremella FUCIFORMIS) extract; 4.00% glycerol; 1.00% sorbitol; water (make up to 100%);
phase II: 1.00 percent of wall-broken yeast extract; and adjusting the pH =7 by using proper amount of citric acid and potassium hydroxide.
Experimental strains
Escherichia coli (Escherichia coli), pseudomonas cepacia (Pseudomonas cepacia), pseudomonas aeruginosa (Pseudomonas aeruginosa), staphylococcus Aureus (Staphylococcus Aureus), aspergillus niger (Aspergillus niger), and Candida albicans (Candida albicans).
Experimental reagent
Tryptone soy broth, yeast malt extract medium, letheen broth, lecithin tween medium, and Bengal red medium.
Pretreatment of the experiment
The concentration of bacteria (Escherichia coli, pseudomonas cepacia, pseudomonas aeruginosa and Staphylococcus aureus) was 10 8 The addition concentration of mould (Aspergillus niger) and yeast (Candida albicans) is 10% 7 And (4) the concentration is/ml. The experimental recording time points were day 2, 7, 14, 21, 28 respectively after the start of the experiment, with repeated challenges on day 21.
TABLE 8 results of the experiment
Conclusion of the experiment
From tables 7 and 8, it can be seen that: all samples passed the preservative challenge test, demonstrating that the compound preservative is effective in preserving at different production temperatures.
EXAMPLE 6 stability study of a composite preservative
Randomly selecting a plurality of anticorrosion combinations; the stability of the compound preservative is verified through high-low temperature and accelerated tests.
TABLE 9 test samples
| Sample numbering | Anti-corrosion ratio |
| 1 | 30% of p-hydroxyacetophenone; 1% caprylyl glycol; 10% hexylene glycol; 59% of dipropylene glycol |
| 2 | 15% of p-hydroxyacetophenone; 10% caprylyl glycol; 50% hexylene glycol; 25% dipropylene glycol |
| 3 | 30% of p-hydroxyacetophenone; 1% glyceryl caprylate; 10% hexylene glycol; 59% dipropylene glycol |
| 4 | 15% of p-hydroxyacetophenone; 10% glyceryl caprylate; 50% hexylene glycol; 25% dipropylene glycol |
TABLE 10 stability test Environment
TABLE 11 results of the experiment
TABLE 12 conclusion of the experiments
As can be seen from tables 9 to 12, the compound preservative of the present invention is stable at both high and low temperatures.
Example 7 Studies of dipropylene glycol as an effective solvent for composite preservatives
As described in the background art, the use of p-hydroxyacetophenone as an alternative preservative is faced with the technical difficulty of dissolution: although p-hydroxyacetophenone can be easily dissolved and stabilized using a conventional effective solubilizer, the solubilizer itself poses safety risks and is not popular with consumers and the market. In the list of chemicals allowed by personal care industry regulations, after a series of possible alternative solvents are screened and discharged (mainly alcohol substances with similar molecular weight and molecular structure to dipropylene glycol) after basic dissolution compatibility analysis by considering feasibility factors of finished products, the dissolution research of p-hydroxyacetophenone is carried out as follows.
The experimental method comprises the following steps:
preparing a 30% (volume percentage) p-hydroxyacetophenone solution by mixing the target solvent with p-hydroxyacetophenone at a ratio of 7: fully dissolving and stirring the mixture for 30 minutes at the water bath temperature of 80 ℃, placing the solution into a constant temperature box at the temperature of 4 ℃, standing the solution, and taking out each solution after one month to observe the state of the solution.
The selected target solvents are as follows: dipropylene glycol, 1, 3-propanediol, 1, 3-butanediol, methyl propanediol, isoprene glycol and water. As can be seen from FIG. 1, several other solvents, except dipropylene glycol, exhibited varying degrees of p-hydroxyacetophenone precipitation; the dipropylene glycol still keeps a clear and transparent state, and the dipropylene glycol is proved to be a safe and effective p-hydroxyacetophenone solvent.
Claims (36)
1. The application of the composition as a composite preservative in cosmetics is characterized in that the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of octyl glycol and/or glyceryl caprylate, 5 to 55 percent of hexanediol and/or isoprene glycol, and dipropylene glycol; wherein dipropylene glycol is used to make up to 100%.
2. The use according to claim 1, wherein the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of octyl glycol and/or glyceryl caprylate, 5 percent of isoprene glycol and dipropylene glycol;
or the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of caprylic glycol and/or caprylic glyceride, 10 to 50 percent of hexanediol and dipropylene glycol;
or, the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of caprylic glycol and/or caprylic glyceride, 1 to 5 percent of isoprene glycol, 10 to 50 percent of hexanediol and dipropylene glycol.
3. The application of claim 2, wherein the mass percent of the p-hydroxyacetophenone is 15% -22% or 22% -30%;
the mass percent of the caprylic glycol and/or caprylic glyceride is 1-6% or 6-10%;
and/or the mass percent of the hexanediol is 5-30% or 30-50%.
4. The use as claimed in claim 3, wherein the mass percentage of p-hydroxyacetophenone is 22%;
the mass percent of the caprylic glycol and/or caprylic glycerol is 6 percent;
and/or the mass percent of the hexanediol is 30%.
5. The use of claim 3, wherein the composition further comprises an adjunct component comprising one or more of pentane diol, 1, 3-butane diol, and 1, 3-propane diol.
6. The use according to claim 5, wherein the composition comprises the following components in percentage by mass: 22% of p-hydroxyacetophenone, 6% of caprylic glycol and/or caprylic glyceride and 30% of hexylene glycol, with dipropylene glycol to make up to 100%;
or 30% of p-hydroxyacetophenone, 1% of octyl glycol, 10% of hexanediol and 1% of isoprene glycol, and the balance being dipropylene glycol to 100%;
or 15% of p-hydroxyacetophenone, 10% of glyceryl caprylate and 50% of hexylene glycol, and the balance being dipropylene glycol to 100%; or 30% of p-hydroxyacetophenone, 1% of glyceryl caprylate and 10% of hexylene glycol, and the balance being dipropylene glycol to 100%;
or 15% of p-hydroxyacetophenone, 10% of octanediol and 50% of hexanediol, with dipropylene glycol to make up to 100%;
or 30% of p-hydroxyacetophenone, 1% of caprylyl glycol and 10% of hexylene glycol, and the balance is dipropylene glycol to 100%; or 30% of p-hydroxyacetophenone, 10% of glyceryl caprylate and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 30% of p-hydroxyacetophenone, 10% of octyl glycol and 5% of isoprene glycol, and the dipropylene glycol is used for complementing to 100%;
or 15% of p-hydroxyacetophenone, 10% of glyceryl caprylate, 50% of hexanediol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 30% of p-hydroxyacetophenone, 1% of glyceryl caprylate, 10% of hexanediol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 15% of p-hydroxyacetophenone, 10% of caprylyl glycol, 50% of hexylene glycol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 30% of p-hydroxyacetophenone, 1% of caprylyl glycol, 10% of hexylene glycol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%.
7. The use according to claim 6, wherein the composition comprises the following components in percentage by mass:
22% p-hydroxyacetophenone, 6% caprylic and/or caprylic glycerol, 30% hexylene glycol, and 42% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% octylene glycol, 10% hexylene glycol, 1% isoprene glycol, and 58% dipropylene glycol;
alternatively, 15% p-hydroxyacetophenone, 10% glyceryl caprylate, 50% hexylene glycol, and 25% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% glyceryl caprylate, 10% hexylene glycol, and 59% dipropylene glycol;
alternatively, 15% p-hydroxyacetophenone, 10% caprylyl glycol, 50% hexylene glycol, and 25% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% caprylyl glycol, 10% hexylene glycol, and 59% dipropylene glycol;
or 30% of p-hydroxyacetophenone, 10% of glyceryl caprylate, 5% of isoprene glycol and 55% of dipropylene glycol;
or 30% of p-hydroxyacetophenone, 10% of caprylyl glycol, 5% of isoprene glycol and 55% of dipropylene glycol;
alternatively, 15% p-hydroxyacetophenone, 10% glyceryl caprylate, 50% hexylene glycol, 5% isoprene glycol, and 20% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% glyceryl caprylate, 10% hexylene glycol, 5% isoprene glycol, and 54% dipropylene glycol;
alternatively, 15% p-hydroxyacetophenone, 10% caprylyl glycol, 50% hexylene glycol, 5% isoprene glycol, and 20% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% caprylyl glycol, 10% hexylene glycol, 5% isoprene glycol, and 54% dipropylene glycol.
8. The use according to any one of claims 1 to 7, wherein the composition is prepared by a process comprising mixing the dipropylene glycol, the hexylene glycol and/or isoprene glycol, and the mixture of caprylic glycol and/or caprylic glyceride with the p-hydroxyacetophenone, and dissolving the mixture under heating.
9. The use according to claim 8, wherein the preparation method comprises the steps of:
(1) Heating and dissolving the mixture of the dipropylene glycol, the hexylene glycol and/or isoprene glycol and the caprylic glycol and/or caprylic glyceride;
(2) Adding the p-hydroxyacetophenone, heating for dissolving, and cooling.
10. The use according to claim 9, wherein the state after dissolution by heating in step (1) is a transparent state.
11. The use of claim 9, wherein the cooled temperature in step (2) is room temperature.
12. The use of claim 1, wherein the composition acts as a compound preservative to inhibit the growth of one or more of bacteria, mold, and yeast.
13. Use according to claim 12, characterized in thatThe bacterium is selected from Escherichia coli (E.coli) (II)Escherichia coli) Pseudomonas cepacia (B)Pseudomonas cepacia) Pseudomonas aeruginosaPseudomonas aeruginosa) And Staphylococcus aureus (StaphylococcusAureus) One or more of (a).
14. The use according to claim 12, wherein the mold is Aspergillus niger (Aspergillus niger)Aspergillus niger）。
15. The use of claim 12, wherein said yeast is candida albicans (candida albicans: (candida albicans))Candida albicans）。
16. The use according to claim 1, wherein the composition is present in the cosmetic product in a concentration of 0.5% to 2%.
17. The use according to claim 16, wherein the concentration is 1.4% to 1.7%, the percentages being by mass.
18. The use of claim 17, wherein said concentration is 1.5%; the percentage is mass percentage.
19. The application of the composition as a composite preservative in skin care products is characterized in that the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of octyl glycol and/or glyceryl caprylate, 5 to 55 percent of hexanediol and/or isoprene glycol, and dipropylene glycol; wherein dipropylene glycol is used to make up to 100%.
20. The use according to claim 19, wherein the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of caprylic glycol and/or caprylic glyceride, 5 percent of isoprene glycol and dipropylene glycol;
or the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of caprylic glycol and/or caprylic glyceride, 10 to 50 percent of hexanediol and dipropylene glycol;
or the composition comprises the following components in percentage by mass: 15 to 30 percent of p-hydroxyacetophenone, 1 to 10 percent of octyl glycol and/or glyceryl caprylate, 1 to 5 percent of isoprene glycol, 10 to 50 percent of hexanediol and dipropylene glycol.
21. The application of claim 20, wherein the mass percent of the p-hydroxyacetophenone is 15% -22% or 22% -30%;
the mass percent of the caprylic glycol and/or the caprylic glyceride is 1-6% or 6-10%;
and/or the mass percent of the hexanediol is 5-30% or 30-50%.
22. The use of claim 21, wherein the mass percent of p-hydroxyacetophenone is 22%;
the mass percent of the caprylic glycol and/or caprylic glycol is 6%;
and/or the mass percent of the hexanediol is 30%.
23. The use of claim 21, wherein the composition further comprises an adjunct component comprising one or more of pentane diol, 1, 3-butane diol, and 1, 3-propane diol.
24. The use according to claim 23, wherein the composition comprises the following components in percentage by mass: 22% of p-hydroxyacetophenone, 6% of caprylic glycol and/or caprylic glyceride and 30% of hexylene glycol, with dipropylene glycol to make up to 100%;
or 30% of p-hydroxyacetophenone, 1% of caprylyl glycol, 10% of hexylene glycol and 1% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 15% of p-hydroxyacetophenone, 10% of glyceryl caprylate and 50% of hexylene glycol, and the balance being dipropylene glycol to 100%; or 30% of p-hydroxyacetophenone, 1% of glyceryl caprylate and 10% of hexylene glycol, and the balance being dipropylene glycol to 100%;
or 15% of p-hydroxyacetophenone, 10% of octanediol and 50% of hexanediol, the balance being dipropylene glycol to 100%;
or 30% of p-hydroxyacetophenone, 1% of caprylyl glycol and 10% of hexylene glycol, and the balance is dipropylene glycol to 100%; or 30% of p-hydroxyacetophenone, 10% of glyceryl caprylate and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 30% of p-hydroxyacetophenone, 10% of caprylyl glycol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 15% of p-hydroxyacetophenone, 10% of glyceryl caprylate, 50% of hexanediol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 30% of p-hydroxyacetophenone, 1% of glyceryl caprylate, 10% of hexanediol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 15% of p-hydroxyacetophenone, 10% of caprylyl glycol, 50% of hexylene glycol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%;
or 30% of p-hydroxyacetophenone, 1% of caprylyl glycol, 10% of hexylene glycol and 5% of isoprene glycol, and the balance is dipropylene glycol to 100%.
25. The use of claim 24, wherein the composition consists of, in mass percent:
22% p-hydroxyacetophenone, 6% caprylic glycol and/or caprylic acid ester, 30% hexylene glycol, and 42% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% caprylyl glycol, 10% hexylene glycol, 1% isoprene glycol, and 58% dipropylene glycol;
alternatively, 15% p-hydroxyacetophenone, 10% glyceryl caprylate, 50% hexylene glycol, and 25% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% glyceryl caprylate, 10% hexylene glycol, and 59% dipropylene glycol;
alternatively, 15% p-hydroxyacetophenone, 10% caprylyl glycol, 50% hexylene glycol, and 25% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% caprylyl glycol, 10% hexylene glycol, and 59% dipropylene glycol;
or 30% of p-hydroxyacetophenone, 10% of glyceryl caprylate, 5% of isoprene glycol and 55% of dipropylene glycol;
or 30% of p-hydroxyacetophenone, 10% of caprylyl glycol, 5% of isoprene glycol and 55% of dipropylene glycol;
alternatively, 15% p-hydroxyacetophenone, 10% glyceryl caprylate, 50% hexylene glycol, 5% isoprene glycol, and 20% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% glyceryl caprylate, 10% hexylene glycol, 5% isoprene glycol, and 54% dipropylene glycol;
alternatively, 15% p-hydroxyacetophenone, 10% caprylyl glycol, 50% hexylene glycol, 5% isoprene glycol, and 20% dipropylene glycol;
alternatively, 30% p-hydroxyacetophenone, 1% caprylyl glycol, 10% hexylene glycol, 5% isoprene glycol, and 54% dipropylene glycol.
26. The use according to any one of claims 19 to 25, wherein the composition is prepared by a process comprising mixing the dipropylene glycol, the hexylene glycol and/or isoprene glycol, and the mixture of caprylic glycol and/or caprylic glyceride with the p-hydroxyacetophenone, and dissolving the mixture under heating.
27. The use of claim 26, wherein the method of making comprises:
(1) Heating and dissolving the mixture of the dipropylene glycol, the hexylene glycol and/or isoprene glycol and the caprylic glycol and/or caprylic glyceride;
(2) Adding the p-hydroxyacetophenone, heating for dissolving, and cooling.
28. The use of claim 27, wherein said heat-dissolved state of step (1) is a transparent state.
29. The use of claim 27, wherein the temperature after cooling in step (2) is room temperature.
30. The use of claim 19, wherein the composition inhibits the growth of one or more of bacteria, mold, and yeast as a compound preservative.
31. The use of claim 30, wherein said bacterium is selected from the group consisting of escherichia coli (h.coli)Escherichia coli) Pseudomonas cepacia (B)Pseudomonas cepacia) Pseudomonas aeruginosaPseudomonas aeruginosa) And Staphylococcus aureus (StaphylococcusAureus) One or more of (a).
32. The use according to claim 30, wherein the mold is Aspergillus niger (Aspergillus niger)Aspergillus niger）。
33. The use of claim 30, wherein said yeast is candida albicans (candida albicans)Candida albicans）。
34. The use of claim 19, wherein said composition is present in said skin care product at a concentration of from 0.5% to 2%.
35. The use of claim 34, wherein the concentration is 1.4% to 1.7%, said percentages being by mass.
36. The use of claim 35, wherein said concentration is 1.5%; the percentage is mass percentage.
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