阅读说明：本技术 一种含对羟基苯乙酮的组合物及其制备方法和应用 (Composition containing p-hydroxyacetophenone and preparation method and application thereof ) 是由 佟月姣 于 2021-10-13 设计创作，主要内容包括：本发明涉及防腐剂技术领域。本发明提供了一种含对羟基苯乙酮的组合物及其制备方法和应用,所述组合物包含如下重量份的组分：对羟基苯乙酮10～40份、C3-C8的二元醇30～70份、植物提取物1～6份。采用本发明的组合物制备的防腐剂安全高效,抑菌谱广,水溶性好,方便使用。既可以单独成为化妆品配方中的防腐体系,也可以与传统防腐剂配伍使用,减少传统防腐剂的用量。也可作为概念上的“无添加”原料,单独应用于产品中,防腐效果良好。同时,不会在各种化妆品中释放甲醛等有害物质,温和不刺激皮肤。(The invention relates to the technical field of preservatives. The invention provides a composition containing p-hydroxyacetophenone, a preparation method and an application thereof, wherein the composition comprises the following components in parts by weight: 10-40 parts of p-hydroxyacetophenone, 30-70 parts of C3-C8 dihydric alcohol and 1-6 parts of plant extract. The preservative prepared by the composition is safe and efficient, has a wide antibacterial spectrum and good water solubility, and is convenient to use. Not only can be independently used as a preservative system in a cosmetic formula, but also can be used together with the traditional preservative, so that the dosage of the traditional preservative is reduced. Can also be used as a conceptual 'no-additive' raw material and is independently applied to products, and the anti-corrosion effect is good. Meanwhile, harmful substances such as formaldehyde and the like cannot be released in various cosmetics, and the skin care product is mild and does not irritate the skin.)

1. The composition containing p-hydroxyacetophenone is characterized by comprising the following components in parts by weight: 10-40 parts of p-hydroxyacetophenone, 30-70 parts of C3-C8 dihydric alcohol and 1-6 parts of plant extract.

2. The composition containing p-hydroxyacetophenone according to claim 1, characterized in that the diol of C3-C8 is one or more of 1, 2-propanediol, 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, 1, 2-octanediol and dipropylene glycol.

3. The composition containing p-hydroxyacetophenone according to claim 1 or 2, characterized in that the plant extract is one or more of grapefruit fruit extract, orange fruit extract, clove flower extract and bitter ginseng root extract.

4. A process for the preparation of a composition according to any one of claims 1 to 3, characterized in that it comprises the following steps: mixing p-hydroxyacetophenone and C3-C8 dihydric alcohol, adding plant extract, and mixing to obtain the final product.

5. The method according to claim 4, wherein the temperature of the mixture of p-hydroxyacetophenone and C3-C8 glycol is 60 to 80 ℃, and the temperature of the mixture after the plant extract is added is 40 to 50 ℃.

6. Use of a composition according to any one of claims 1 to 3 as a cosmetic preservative.

7. Use according to claim 6, characterized in that the cosmetic has a pH value of 3.0 to 9.0.

8. Use according to claim 7, wherein the composition is present in the cosmetic product in an amount of 0.5 to 2.5% by weight.

9. The use of any one of claims 6 to 8, wherein the composition is formulated with phenoxyethanol and/or chlorphenesin.

Technical Field

The invention relates to the technical field of preservatives, and particularly relates to a composition containing p-hydroxyacetophenone, and a preparation method and application thereof.

Background

In recent years, natural raw materials and various functional additives used in the cosmetic industry have been increasing, products are more easily corroded by microorganisms, and preservation of cosmetics has been more and more emphasized. Some of the traditional preservative varieties in the preservative list are always disputed for their safety. Such as formaldehyde and its slow-release agents, isothiazolinones, parabens, IPBC, triclosan, etc., are often pushed to the wind gap sharp of public opinion, so that the consumer's emotional conflict with preservatives is high, and the choice of cosmetic manufacturers is less and less. Consumers are also increasingly recognizing products that are "free of preservatives", "zero added", "no added", etc.

This trend has made the cosmetic raw materials, such as p-hydroxyacetophenone, octanoyl hydroxamic acid, ethylhexyl glycerol, glycols, etc., which are not in the category of preservatives but have a certain preservative efficacy, the focus of attention. The rational and effective use of these materials provides the personal care market with a greater choice of preservative systems within the scope of the regulations, while also improving efficacy by reducing the amount of existing traditional preservative varieties through synergistic effects.

The p-hydroxyacetophenone is extracted from giant knotweed rhizome, cynanchum atratum and other plants, is used as a component of medicaments for benefiting gallbladder, reducing blood fat and the like, and mainly plays a role in the field of medicines. How to develop a safe, high-efficiency and convenient cosmetic bacteriostatic agent by using the bacteriostatic agent is not relevant to research at present.

Disclosure of Invention

The invention aims to provide a composition containing p-hydroxyacetophenone, a preparation method and application thereof, which can reduce the dosage of the traditional preservative.

In order to achieve the above object, the present invention provides the following technical solutions:

the invention provides a composition containing p-hydroxyacetophenone, which comprises the following components in parts by weight: 10-40 parts of p-hydroxyacetophenone, 30-70 parts of C3-C8 dihydric alcohol and 1-6 parts of plant extract.

Preferably, the dihydric alcohol of C3-C8 is one or more of 1, 2-propanediol, 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, 1, 2-octanediol, and dipropylene glycol.

Preferably, the plant extract is one or more of grapefruit fruit extract, orange fruit extract, clove flower extract and sophora flavescens root extract.

The invention also provides a preparation method of the composition, which comprises the following steps: mixing p-hydroxyacetophenone and C3-C8 dihydric alcohol, adding plant extract, and mixing to obtain the final product.

Preferably, the temperature of the mixture of the p-hydroxyacetophenone and the dihydric alcohol of C3-C8 is 60-80 ℃, and the temperature of the mixture of the p-hydroxyacetophenone and the dihydric alcohol of C3-C8 is 40-50 ℃.

The invention also provides the application of the composition as a cosmetic preservative.

Preferably, the pH value of the cosmetic is 3.0-9.0.

Preferably, the content of the composition in the cosmetic is 0.5-2.5 wt%.

Preferably, the composition can be used in combination with phenoxyethanol and/or chlorphenesin.

The invention provides a composition containing p-hydroxyacetophenone, a preparation method and an application thereof, wherein the composition comprises the following components in parts by weight: 10-40 parts of p-hydroxyacetophenone, 30-70 parts of C3-C8 dihydric alcohol and 1-6 parts of plant extract. The preservative prepared by the composition is safe and efficient, has a wide antibacterial spectrum and good water solubility, and is convenient to use. Not only can be independently used as a preservative system in a cosmetic formula, but also can be used together with the traditional preservative, so that the dosage of the traditional preservative is reduced. Can also be used as a conceptual 'no-additive' raw material and is independently applied to products, and the anti-corrosion effect is good. Meanwhile, harmful substances such as formaldehyde and the like cannot be released in various cosmetics, and the skin care product is mild and does not irritate the skin. The composition containing the p-hydroxyacetophenone is suitable for cosmetics such as facial masks, water emulsions and creams, is small in addition amount, is in a liquid state, can reduce the production cost of the cosmetics, is simple and convenient to operate in the using process, but has an outstanding preservative effect, prevents the breeding of microorganisms in the cosmetics, is mild and does not irritate the skin.

Detailed Description

The invention provides a composition containing p-hydroxyacetophenone, which comprises the following components in parts by weight: 10-40 parts of p-hydroxyacetophenone, 30-70 parts of C3-C8 dihydric alcohol and 1-6 parts of plant extract.

In the invention, the preferred part of the p-hydroxyacetophenone is 15 to 35 parts, more preferably 20 to 30 parts, and still more preferably 25 parts.

In the present invention, the proportion of the C3-C8 diol is preferably 40 to 60 parts, more preferably 45 to 55 parts, and still more preferably 50 parts.

In the present invention, the plant extract is preferably 2 to 5 parts, and more preferably 3 to 4 parts.

In the present invention, the dihydric alcohol of C3-C8 is preferably one or more of 1, 2-propanediol, 1, 3-butanediol, 1, 2-pentanediol, 1, 2-hexanediol, 1, 2-octanediol, and dipropylene glycol.

In the present invention, the plant extract is preferably one or more of grapefruit fruit extract, orange fruit extract, clove flower extract and sophora flavescens root extract.

In the invention, when the plant extract simultaneously comprises grapefruit fruit extract, orange fruit extract, clove flower extract and bitter ginseng root extract, the weight ratio of the bitter ginseng root extract to the clove flower extract to the grapefruit fruit extract to the orange fruit extract is 0.2-1.5: 0.6-2.2: 0.6-2: 0.6 to 1.

The invention also provides a preparation method of the composition, which comprises the following steps: mixing p-hydroxyacetophenone and C3-C8 dihydric alcohol, adding plant extract, and mixing to obtain the final product.

In the invention, the temperature of the mixture of the p-hydroxyacetophenone and the dihydric alcohol of C3-C8 is preferably 60-80 ℃, more preferably 65-75 ℃, and even more preferably 70 ℃.

In the present invention, the temperature at the time of mixing after adding the plant extract is preferably 40 to 50 ℃, more preferably 43 to 47 ℃, and still more preferably 45 ℃.

The invention also provides the application of the composition as a cosmetic preservative.

In the present invention, the composition is capable of inhibiting candida albicans, staphylococcus aureus, escherichia coli, pseudomonas aeruginosa or aspergillus niger.

In the present invention, the pH of the cosmetic is preferably 3.0 to 9.0, more preferably 5.0 to 7.0, and still more preferably 6.0.

In the present invention, the content of the composition in the cosmetic is preferably 0.5 to 2.5 wt%, more preferably 1 to 2 wt%, and still more preferably 1.5 wt%.

In the invention, the composition can be matched with phenoxyethanol and/or chlorphenesin for use

The technical solutions provided by the present invention are described in detail below with reference to examples, but they should not be construed as limiting the scope of the present invention.

Example 1 determination of the amount of p-hydroxyacetophenone added

The solubility of p-hydroxyacetophenone is slightly soluble in water, and is easily soluble in ethanol, and in order to realize the maximum solubility of p-hydroxyacetophenone in the antiseptic composition, other solvents except water are screened to be used as the solvent of p-hydroxyacetophenone, and the p-hydroxyacetophenone is prepared into a liquid use form, so that the problem of inconvenient operation in the use process of the p-hydroxyacetophenone is solved.

Solvents commonly used as cosmetic solvents include dipropylene glycol, 1, 3-butylene glycol, ethanol, 1, 3-propylene glycol, and the like. Considering the bad smell of ethanol and the potential influence on the consistency of the product, and considering the price of the raw material, dipropylene glycol was primarily screened as a solvent for dissolving p-hydroxyacetophenone.

The preparation method comprises the following steps: adding p-hydroxyacetophenone and dipropylene glycol into a container according to different proportions, heating to 80 ℃, and uniformly stirring to obtain the composition.

The experimental method comprises the following steps: the obtained compositions were allowed to stand at 20 ℃ and 4 ℃ to-4 ℃ for 24 hours, respectively, and then observed.

The dosage ratio and stability of each component are shown in table 1.

TABLE 1

According to the results shown in Table 1, the sample containing 40% of p-hydroxyacetophenone was further left at room temperature and observed for a long period of time, and it was found that crystals precipitated in the 11 th month after the preparation date of the sample containing 40% of p-hydroxyacetophenone. According to the results of short-term accelerated observation experiment and long-term observation experiment, the maximum solubility of p-hydroxyacetophenone in the dipropylene glycol solution is judged to be between 30% and 40%.

Example 2

The raw materials are weighed according to the weight parts of 30 parts of p-hydroxyacetophenone, 30 parts of 1, 2-hexanediol, 38 parts of dipropylene glycol, 0.2 part of sophora flavescens root extract, 0.6 part of clove extract, 0.6 part of grapefruit extract and 0.6 part of orange extract.

Heating p-hydroxyacetophenone and dipropylene glycol at 70 deg.C under stirring for dissolving, adding 1, 2-hexanediol under stirring at 40 deg.C, and adding plant extract under stirring at 45 deg.C to obtain antiseptic containing p-hydroxyacetophenone, wherein the pH is 4.67, and the antiseptic containing p-hydroxyacetophenone has stable property.

The p-hydroxyacetophenone-containing preservative can be added to 1.5 wt% of an ointment cosmetic, the pH of the ointment cosmetic is 4.67, and the ointment cosmetic has stable properties.

Example 3

The raw materials are weighed according to the weight parts of 30 parts of p-hydroxyacetophenone, 30 parts of 1, 2-hexanediol, 37 parts of dipropylene glycol, 1.2 parts of sophora flavescens root extract, 0.6 part of clove extract, 0.6 part of grapefruit extract and 0.6 part of orange extract.

Heating and stirring p-hydroxyacetophenone and dipropylene glycol at 80 deg.C to dissolve, stirring at 45 deg.C to add 1, 2-hexanediol, and stirring at 45 deg.C to add plant extract to obtain antiseptic containing p-hydroxyacetophenone, wherein the pH is 5.06, and the antiseptic containing p-hydroxyacetophenone has stable property.

The p-hydroxyacetophenone-containing preservative can be added to 1.0 wt% of an ointment cosmetic, the pH of the ointment cosmetic is 5.06, and the ointment cosmetic has stable properties.

Example 4

The raw materials are weighed according to the weight parts of 30 parts of p-hydroxyacetophenone, 30 parts of 1, 2-hexanediol, 34 parts of dipropylene glycol, 1.0 part of sophora flavescens root extract, 2.2 parts of clove extract, 2.0 parts of grapefruit extract and 0.8 part of orange extract.

Heating p-hydroxyacetophenone and dipropylene glycol at 60 deg.C under stirring for dissolving, adding 1, 2-hexanediol at 50 deg.C under stirring, and adding plant extract at 50 deg.C under stirring to obtain antiseptic containing p-hydroxyacetophenone with pH of 5.08, wherein the antiseptic containing p-hydroxyacetophenone has stable property.

The p-hydroxyacetophenone-containing preservative can be added to 2.5 wt% of an ointment cosmetic, the pH of the ointment cosmetic is 5.08, and the ointment cosmetic has stable properties.

Comparative example 1

Weighing the raw materials according to the weight parts of 35 parts of p-hydroxyacetophenone, 30 parts of 1, 2-hexanediol and 35 parts of dipropylene glycol.

Heating and stirring p-hydroxyacetophenone and dipropylene glycol at 80 deg.C to dissolve, stirring and adding 1, 2-hexanediol at 50 deg.C to obtain the antiseptic containing p-hydroxyacetophenone, wherein crystal is precipitated after one week of preparation.

Comparative example 2

Weighing the raw materials according to the weight parts of 30 parts of p-hydroxyacetophenone, 30 parts of 1, 2-hexanediol and 40 parts of water.

Heating p-hydroxyacetophenone and water at 80 deg.C, stirring for dissolving, adding 1, 2-hexanediol at 50 deg.C under stirring to obtain the antiseptic containing p-hydroxyacetophenone, and layering.

Comparative example 3

The raw materials are weighed according to the weight parts of 30 parts of p-hydroxyacetophenone, 30 parts of 1, 2-hexanediol, 33.5 parts of dipropylene glycol, 1.5 parts of sophora flavescens root extract, 2.0 parts of clove flower extract, 2.0 parts of grapefruit fruit extract and 1.0 part of orange fruit extract.

Heating p-hydroxyacetophenone and dipropylene glycol at 80 deg.C under stirring for dissolving, adding 1, 2-hexanediol at 50 deg.C under stirring, adding plant extract at 45 deg.C under stirring to obtain p-hydroxyacetophenone-containing preservative with pH of 5.12, wherein the obtained p-hydroxyacetophenone-containing preservative has stable properties but the color of the final composition is too dark. Too dark a color of the composition may limit the use of the composition in some colorless, transparent products.

The p-hydroxyacetophenone-containing preservative can be added to 1.5 wt% of an ointment cosmetic, the pH of the ointment cosmetic is 5.12, and the ointment cosmetic has stable properties.

Application example 1

Example 4 was applied to cream cosmetics, and the formulation is shown in table 2:

TABLE 2

The preparation process of the cream cosmetic comprises the following steps:

a. adding the phase A components into an emulsifying pot, heating to 80 ℃, stirring for 30 minutes, and homogenizing for 2 minutes to uniformly disperse carbomer;

b. adding the components of the phase B into an oil phase pot, heating to 80 ℃, and stirring until the components are completely dissolved;

c. pumping the phase B into an emulsifying pot while stirring until the phase B is completely pumped into the emulsifying pot, and homogenizing for 3 minutes;

d. homogenizing in an emulsifying pot for 3 min, introducing cooling water into a jacket, cooling to 50 deg.C, adding phase C, and homogenizing for 3 min;

e. cooling to 45 deg.C, heating phase D, and homogenizing for 3 min;

f. continuously stirring and cooling to 30 ℃ to form cream.

Application example 2

Example 4 was applied to a lotion, the formulation shown in table 3:

TABLE 3

The preparation process of the toning lotion comprises the following steps:

a. putting the phase A component into a preparation tank, stirring and dispersing at 200rpm until all the components are fully dissolved;

b. heating the phase B component to 45 ℃ until all components are dissolved, putting the phase B component into a preparation tank, stirring at 200rpm for 3 minutes;

c. dissolving the phase C component with warm water, putting into a preparation tank, stirring at 200rpm for 3 minutes;

d. uniformly stirring the phase D component, putting the phase D component into a preparation tank, and stirring for 3 minutes at 200 rpm;

and e.400mesh filtering to complete the making process.

As a result: testing of corrosion protection efficacy

A 28 day single inoculation challenge test was performed with reference to the preservative system efficacy evaluation method recommended by the american cosmetic perfume flavor association (CTFA).

1. Test strains: bacteria (escherichia coli, staphylococcus aureus, pseudomonas aeruginosa); fungi (aspergillus niger, candida albicans). Mixed bacteria are adopted for inoculation.

2. Test samples: according to the formulas and the processes in the tables 2 and 3, a cosmetic cream formula and a lotion formula are respectively prepared, and a preservative challenge experiment is carried out to investigate the preservative effect of the preservative composition containing p-hydroxyacetophenone in different cosmetic systems.

3. The result shows that the preservative composition containing the p-hydroxyacetophenone can play a role in preserving and inhibiting bacteria when being used in daily chemical products independently; the preservative can also be compounded with a small amount of traditional preservatives for use, and the formula can play a role in reducing the addition of the traditional preservatives.

From the above examples, the present invention provides a composition containing p-hydroxyacetophenone, a preparation method and applications thereof, wherein the composition comprises the following components by weight: 10-40 parts of p-hydroxyacetophenone, 30-70 parts of C3-C8 dihydric alcohol and 1-6 parts of plant extract. The preservative prepared by the composition is safe and efficient, has a wide antibacterial spectrum and good water solubility, and is convenient to use. Not only can be independently used as a preservative system in a cosmetic formula, but also can be used together with the traditional preservative, so that the dosage of the traditional preservative is reduced. Can also be used as a conceptual 'no-additive' raw material and is independently applied to products, and the anti-corrosion effect is good. Meanwhile, harmful substances such as formaldehyde and the like cannot be released in various cosmetics, and the skin care product is mild and does not irritate the skin. The composition containing the p-hydroxyacetophenone is suitable for cosmetics such as facial masks, water emulsions and creams, is small in addition amount, is in a liquid state, can reduce the production cost of the cosmetics, is simple and convenient to operate in the using process, but has an outstanding preservative effect, prevents the breeding of microorganisms in the cosmetics, is mild and does not irritate the skin.

The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.