CN113197789A

CN113197789A - Astaxanthin antioxidant essence milk with stable quality and preparation method thereof

Info

Publication number: CN113197789A
Application number: CN202110487513.XA
Authority: CN
Inventors: 张慧; 林娜妹; 张金金; 李传茂; 张伟杰; 张楚标
Original assignee: Guangdong Danz Group Co Ltd; Guangzhou Keneng Cosmetic Research Co Ltd
Current assignee: Guangdong Danz Group Co Ltd; Guangzhou Keneng Cosmetic Research Co Ltd
Priority date: 2021-04-30
Filing date: 2021-04-30
Publication date: 2021-08-03

Abstract

The invention relates to the technical field of cosmetics and discloses astaxanthin antioxidant essence milk with stable quality and a preparation method thereof. The essence milk comprises the following components in percentage by mass: 0.001-0.5% of astaxanthin; polyol: 2 to 20 percent; antioxidant: 0.01-1%; 0.01-10% of skin conditioner; chelating agent: 0.01-1%; thickening agent: 0.01-1%; pH regulators: 0.01-1%; 0.1-20% of grease; emulsifier: 0.01 to 5 percent; preservative: 0.05-2%; 50-80% of water. According to the invention, through combination of the antioxidant component and the emulsion dispersion system, the astaxanthin in the component is effectively protected, so that the astaxanthin keeps excellent antioxidant effect, plays a role in the essence milk, and effectively reduces the damage of free radicals to human skin.

Description

Astaxanthin antioxidant essence milk with stable quality and preparation method thereof

Technical Field

The invention belongs to the technical field of cosmetics, and particularly relates to astaxanthin antioxidant essence milk with stable quality and a preparation method thereof.

Background

Free radicals are intermediate metabolites of various biochemical reactions in human life activities, have high chemical activity, are effective defense systems of organisms, and influence the life activities of the organisms if the free radicals cannot maintain a certain level. However, the radicals are produced too much to be removed in time, and then attack the living macromolecular substances and various organelles in the body, causing various damages of the body at molecular level, cellular level and tissue and organ level, accelerating the aging process of the body and inducing various diseases.

Astaxanthin is one of carotenoids, a strong natural antioxidant. The capacity of the compound to remove free radicals is 10 times that of lycopene, 100 times that of beta-carotene, 700 times that of anthocyanin, 1000 times that of vitamin E and 6000 times that of vitamin C. The aging of the human body is mainly caused by oxidation caused by free radicals. The special molecular structure of astaxanthin can penetrate through the outer wall of human cells, directly remove oxygen free radicals in the cells, enhance the regeneration capacity of the cells, maintain the functional balance of the human body, reduce the accumulation of aged cells and protect the health of the cells and DNA from inside to outside. But astaxanthin has poor stability and easy color fading, and the service life and the effectiveness of the astaxanthin are seriously influenced.

Disclosure of Invention

In view of the defects of the prior art, the invention aims to provide astaxanthin antioxidant essence milk with stable quality and a preparation method of the composition.

According to the first aspect, the invention provides astaxanthin antioxidant essence milk with stable quality, which comprises the following components in percentage by mass: 0.001-0.5% of astaxanthin; polyol: 2 to 20 percent; antioxidant: 0.01-1%; 0.01-10% of skin conditioner; chelating agent: 0.01-1%; thickening agent: 0.01-1%; pH regulators: 0.01-1%; 0.1-20% of grease; emulsifier: 0.01 to 5 percent; preservative: 0.05-2%; 50-80% of water.

In a preferred technical scheme, the astaxanthin is natural organic astaxanthin.

As a preferable technical scheme, the polyalcohol is one or more selected from propylene glycol, butanediol, glycerol and pentanediol.

As a preferable technical scheme, the antioxidant is selected from one or more of sodium metabisulfite, tocopherol and tocopherol acetate.

As a preferable technical scheme, the skin conditioning agent is one or more of allantoin, sodium hyaluronate, sodium PCA, hydrolyzed collagen and hydrolyzed sclerotium rolfsii gum.

As a preferable technical scheme, the chelating agent is selected from one or more of EDTA-2Na and EDTA-4 Na.

As a preferable technical scheme, the thickening agent is selected from one or more of xanthan gum, carrageen crispa, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, acryloyl dimethyl taurate/VP copolymer, hydroxyethyl acrylate/acryloyl dimethyl taurate copolymer and hydroxyethyl cellulose.

As a preferred technical scheme, the PH regulator is selected from one or more of citric acid, sodium citrate, triethanolamine and aminomethyl propanol.

As a preferable technical scheme, the grease is selected from one or more of hydrogenated polyisobutene, dioctyl carbonate, isohexadecane, isononyl isononanoate and caprylic/capric triglyceride.

As a preferable technical scheme, the emulsifier is one or more selected from sorbitan stearate, polysorbate-60, PEG-100 stearate and glycerol stearate.

As a preferable technical scheme, the preservative is selected from one or more of methyl hydroxybenzoate, propyl hydroxybenzoate, phenoxyethanol, ethylhexyl glycerol and p-hydroxyacetophenone.

In the invention, based on that the astaxanthin is unstable under illumination and is easy to be oxidized and faded, the sodium metabisulfite and the tocopherol ethylhexyl ester have good oxidation resistance, and the sodium metabisulfite and the tocopherol ethylhexyl ester can be synergistic and preferentially react with oxygen under illumination, so that the astaxanthin is well protected, and the phenomenon of fading under illumination is relieved.

Meanwhile, the emulsion is a multi-dispersion system, and incident light can be reflected, scattered and transmitted on the surface of the liquid beads due to different refractive indexes of a dispersed phase and a dispersion medium. The particle size of the liquid bead of the emulsion is 0.1-10 μm, and the wavelength of visible light is 0.4-0.6 μm, so the emulsion mainly generates reflection phenomenon. When the astaxanthin essence milk is irradiated by light, most of the light cannot penetrate through the emulsion due to light reflection of the emulsion, so that the astaxanthin is protected, and the damage of the light to the astaxanthin is reduced.

According to the invention, through combination of the antioxidant component and the emulsion dispersion system, the astaxanthin in the component is effectively protected, so that the astaxanthin keeps excellent antioxidant effect, plays a role in the essence milk, and effectively reduces the damage of free radicals to human skin.

In a second aspect, the invention provides a preparation method of astaxanthin antioxidant essence milk with stable quality, which comprises the following steps:

s1, mixing water, a skin conditioner, a thickening agent, an antioxidant and a chelating agent in proportion, stirring and heating to 70-88 ℃ to obtain a mixed solution 1;

s2, mixing the grease and the emulsifier, and heating to 70-88 ℃ to obtain a mixed solution 2;

s3, slowly adding the mixed solution 2 into the mixed solution 1, homogenizing for 3-10min, preserving heat for 15-25min, and cooling to 45 ℃ to obtain a mixed solution 3;

s4, mixing astaxanthin and polyhydric alcohol in proportion and homogenizing for 3-8min to obtain a mixed solution 4;

s5, slowly adding the mixed solution 4, the preservative and the PH regulator into the mixed solution 3, and uniformly stirring to obtain the antioxidant essence milk.

The invention has the beneficial effects that:

according to the invention, on one hand, the sodium metabisulfite and the tocopherol ethylhexyl ester used in the preparation method can be synergistic, so that the light stability of the astaxanthin is protected, on the other hand, the prepared essence milk can reflect light, the damage of the astaxanthin caused by illumination is reduced, the light stability of the astaxanthin is further protected, the prepared astaxanthin essence milk keeps excellent antioxidant effect, and the damage of free radicals to the skin of a human body can be effectively reduced.

Detailed Description

Embodiments of the present invention will be described in detail below with reference to examples, but those skilled in the art will appreciate that the following examples are only illustrative of the present invention and should not be construed as limiting the scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products commercially available.

Example 1

According to the mass percentages of the components in the following table 1, the astaxanthin antioxidant essence milk with stable quality of the example 1 is prepared.

TABLE 1

The preparation method comprises the following steps:

s1, mixing water, sodium hyaluronate, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, sodium metabisulfite, tocopherol ethylhexyl ester and EDTA-2Na in proportion, stirring and heating to 78 ℃ to obtain a mixed solution 1;

s2, mixing isononyl isononanoate, caprylic/capric triglyceride, polysorbate-60 and sorbitan stearate, and heating to 78 ℃ to obtain a mixed solution 2;

s3, slowly adding the mixed solution 2 into the mixed solution 1, homogenizing for 5min, preserving heat for 25min, and cooling to 45 ℃ to obtain a mixed solution 3;

s4, mixing astaxanthin, pentanediol and glycerol in proportion and homogenizing for 7min to obtain a mixed solution 4;

s5, slowly adding the mixed solution 4, phenoxyethanol, methylparaben and aminomethyl propanol into the mixed solution 3, and uniformly stirring to obtain the antioxidant essence milk.

Example 2

According to the mass percentages of the components in the following table 2, the astaxanthin antioxidant essence milk with stable quality of the example 2 is prepared.

TABLE 2

The preparation method comprises the following steps:

s1, mixing water, sodium hyaluronate, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, sodium metabisulfite, tocopherol ethylhexyl ester and EDTA-2Na in proportion, stirring and heating to 85 ℃ to obtain a mixed solution 1;

s2, mixing isononyl isononanoate, caprylic/capric triglyceride, polysorbate-60 and sorbitan stearate, and heating to 85 ℃ to obtain a mixed solution 2;

s3, slowly adding the mixed solution 2 into the mixed solution 1, homogenizing for 6min, preserving heat for 15min, and cooling to 45 ℃ to obtain a mixed solution 3;

s4, mixing astaxanthin, pentanediol and glycerol in proportion and homogenizing for 5min to obtain a mixed solution 4;

Example 3

According to the mass percentages of the components in the following table 3, the astaxanthin antioxidant essence milk with stable quality of the example 3 is prepared.

TABLE 3

Components	The addition ratio%
		Water (W)	Balance of
Pentanediol	2
		Glycerol	3
Hyaluronic acid sodium salt	0.05
		Acrylic acid (ester)/C10-30 alkanol acrylate crosspolymer	0.25
Hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer	0.3
		Sodium metabisulfite	0.05
Tocopherol ethylhexyl ester	0.7
		EDTA-2Na	0.02
Astaxanthin	0.01
		Isononyl isononanoate	4
Caprylic/capric triglyceride	2
		Polysorbate-60	0.8
Sorbitan stearate	0.2
		Aminomethyl propanol	0.12
Phenoxyethanol	0.5
		Hydroxy phenyl methyl ester	0.3

The preparation method comprises the following steps:

s1, mixing water, sodium hyaluronate, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, hydroxyethyl acrylate/sodium acryloyldimethyl taurate copolymer, sodium metabisulfite, tocopherol ethylhexyl ester and EDTA-2Na in proportion, stirring and heating to 83 ℃ to obtain a mixed solution 1;

s2, mixing isononyl isononanoate, caprylic/capric triglyceride, polysorbate-60 and sorbitan stearate, and heating to 83 ℃ to obtain a mixed solution 2;

s3, slowly adding the mixed solution 2 into the mixed solution 1, homogenizing for 5min, preserving heat for 20min, and cooling to 45 ℃ to obtain a mixed solution 3;

Example 4

According to the mass percentages of the components in the following table 4, the astaxanthin antioxidant essence milk with stable quality of the example 4 is prepared.

TABLE 4

Components	The addition ratio%
		Water (W)	Balance of
Pentanediol	2
		Glycerol	3
Hyaluronic acid sodium salt	0.05
		Xanthan gum	0.05
Chondrus crispus (Chondrus crispus)	0.48
		PCA sodium salt	1.5
Sodium metabisulfite	0.05
		Tocopherol ethylhexyl ester	0.7
EDTA-2Na	0.02
		Astaxanthin	0.01
Isononyl isononanoate	4
		Caprylic/capric triglyceride	2
Polysorbate-60	0.8
		Sorbitan stearate	0.2
Citric acid	0.01
		Citric acid sodium salt	0.05
Phenoxyethanol	0.5
		Hydroxy phenyl methyl ester	0.3

The preparation method comprises the following steps:

s1, mixing water, sodium hyaluronate, xanthan gum, carrageen crispa, sodium PCA, sodium metabisulfite, tocopherol ethylhexyl ester and EDTA-2Na in proportion, stirring and heating to 82 ℃ to obtain a mixed solution 1;

s2, mixing isononyl isononanoate, caprylic/capric triglyceride, polysorbate-60 and sorbitan stearate, and heating to 82 ℃ to obtain a mixed solution 2;

s3, slowly adding the mixed solution 2 into the mixed solution 1, homogenizing for 5min, preserving heat for 23min, and cooling to 43 ℃ to obtain a mixed solution 3;

s5, slowly adding the mixed solution 4, phenoxyethanol, methylparaben, citric acid and sodium citrate into the mixed solution 3, and uniformly stirring to obtain the antioxidant essence milk.

Example 5

According to the mass percentages of the components in the following table 5, the astaxanthin antioxidant essence milk with stable quality of the example 5 is prepared.

TABLE 5

The preparation method comprises the following steps:

s1, mixing water, sodium hyaluronate, xanthan gum, carrageen crispa, sodium PCA, sodium metabisulfite, tocopherol ethylhexyl ester and EDTA-2Na in proportion, stirring and heating to 84 ℃ to obtain a mixed solution 1;

s2, mixing isohexadecane, caprylic/capric triglyceride, polysorbate-60 and sorbitan stearate, and heating to 84 ℃ to obtain a mixed solution 2;

s3, slowly adding the mixed solution 2 into the mixed solution 1, homogenizing for 5min, preserving heat for 18min, and cooling to 40 ℃ to obtain a mixed solution 3;

Example 6

According to the mass percentages of the components in the following table 6, the astaxanthin antioxidant essence milk with stable quality of the example 6 is prepared.

TABLE 6

The preparation method comprises the following steps:

s2, mixing isohexadecane, caprylic/capric triglyceride, polysorbate-60 and sorbitan stearate, and heating to 82 ℃ to obtain a mixed solution 2;

s3, slowly adding the mixed solution 2 into the mixed solution 1, homogenizing for 4min, preserving heat for 20min, and cooling to 45 ℃ to obtain a mixed solution 3;

s4, mixing astaxanthin, pentanediol and butanediol in proportion and homogenizing for 5min to obtain a mixed solution 4;

s5, slowly adding the mixed solution 4, phenoxyethanol, ethylhexylglycerin, citric acid and sodium citrate into the mixed solution 3, and uniformly stirring to obtain the antioxidant essence milk.

Example 7

According to the mass percentages of the components in the following table 7, the astaxanthin antioxidant essence milk with stable quality of the example 7 is prepared.

TABLE 7

The preparation method comprises the following steps:

s1, mixing water, allantoin, sodium hyaluronate, xanthan gum, carrageen crispa, sodium PCA, sodium metabisulfite, tocopherol ethylhexyl ester and EDTA-4Na in proportion, stirring and heating to 80 ℃ to obtain a mixed solution 1;

s2, mixing isohexadecane, caprylic/capric triglyceride, polysorbate-60 and sorbitan stearate, and heating to 80 ℃ to obtain a mixed solution 2;

s3, slowly adding the mixed solution 2 into the mixed solution 1, homogenizing for 5min, preserving heat for 20min, and cooling to 40 ℃ to obtain a mixed solution 3;

Comparative examples 1 to 3

The difference between comparative example 1 and example 1 is that comparative example 1 does not add sodium metabisulphite.

The difference between comparative example 2 and example 1 is that tocopherol ethylhexyl ester was not added.

The difference between comparative example 3 and example 1 is that no oil phase ingredients are added for emulsification.

Comparative examples 1-2 were prepared in the same manner as in example 1.

The preparation method of comparative example 3 is as follows:

s2, homogenizing the mixed solution 1 for 5min, keeping the temperature for 25min, and cooling to 45 ℃;

s3, mixing astaxanthin, pentanediol and glycerol in proportion and homogenizing for 7min to obtain a mixed solution 2;

s5, slowly adding the mixed solution 2, phenoxyethanol, methyl hydroxybenzoate and aminomethyl propanol into the mixed solution 1, and uniformly stirring to obtain the comparative example 3.

Test of Experimental Effect

Stability test experiment

The essential milks prepared from the components of examples 1 to 3 and comparative examples 1 to 3 were subjected to high temperature/low temperature/light/xenon lamp/cold heat cycle test, and the change in odor and appearance color of the product under each test condition was monitored to determine the stability of the product, with the results shown in table 8.

TABLE 8

As can be seen from Table 8, after the stability test for 3 months, the quality indexes of examples 1-3 all meet the requirements, and the sodium metabisulfite is not added in comparative example 1, so that the odor is not abnormal, and the appearance shows that the astaxanthin has obvious fading phenomenon in 1 month; comparative example 2 no tocopherol ethylhexyl ester was added, no odor was noted, and the appearance showed significant discoloration of astaxanthin at 1 month; comparative example 3 is a non-emulsified system with no odor abnormality and the appearance shows that astaxanthin undergoes significant discoloration at 14 days and almost complete color fading at 1 month.

Oxidation resistance test

Samples prepared from the components of examples 1 to 3 and comparative examples 1 to 3 were subjected to a stability test for 3 months and then subjected to an oxidation resistance test. The specific evaluation indexes include: DPPH free radical clearance rate, superoxide free radical clearance rate, hydroxyl free radical clearance rate.

1. DPPH radical clearance: 0.04mg/ml of 1, 1-diphenyl-2-trinitrophenylhydrazine solution (DPPH) was prepared using absolute ethanol, 2ml of each of the samples prepared in examples 1 to 3 and comparative examples 1 to 3 was added to 2ml of the DPPH solution, and reacted at room temperature for 30min, with absolute ethanol as a blank, and the absorbance value of the sample at 517nm was measured. DPPH radical clearance was calculated according to the formula [1- (sample/blank) 100% ].

2. Superoxide radical clearance: 50mmol/L Tris-HCl buffer solution is prepared and kept stand for 20min at room temperature. 1ml of the samples prepared in examples 1 to 3 and comparative examples 1 to 3 were added to 4.5ml of Tris-HCl buffer, 0.4ml of 25mmol/L pyrogallol solution was added, the mixture was mixed well and reacted at room temperature for 5min,1ml of HCl was used for the reaction, and the absorbance value of the sample at 299nm was measured using distilled water as a blank. Superoxide radical clearance was calculated according to the formula [ (blank absorbance-sample absorbance)/blank absorbance) × 100% ].

3. Hydroxyl radical scavenging rate: a9 mmol/L salicylic acid solution was prepared in absolute ethanol, 1ml of a 9mmol/L ferric sulfate solution was added, 1ml of the sample prepared in examples 1-3 and comparative examples 1-3 was added, and finally 1ml of a 8.8mmol/L hydrogen peroxide solution was added, and the absorbance value of the sample at 510nm was measured using distilled water as a blank. Hydroxyl radical clearance was calculated according to the formula [1- (absorbance of sample/absorbance of blank control). times.100% ].

The specific evaluation results are shown in table 9 below.

TABLE 9

As can be seen from Table 9, after 3 months of stability test, examples 1-3 all have strong scavenging ability to DPPH free radical, superoxide free radical and hydroxyl free radical, wherein the radical scavenging ability of example 1 is strongest, which indicates that examples 1-3 all have strong antioxidant ability and example 1 has strongest antioxidant ability; the clearance rates of comparative examples 1-3 to DPPH free radicals, superoxide free radicals and hydroxyl free radicals are obviously reduced compared with example 1, and the antioxidant capacity of the comparative examples 1-3 is obviously weakened compared with example 1.

The above description is only for the specific embodiments of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art can easily conceive of the changes or substitutions within the technical scope of the present invention, and the present invention shall be covered thereby. Therefore, the protection scope of the present invention shall be subject to the protection scope of the appended claims.

Claims

1. The astaxanthin antioxidant essence milk with stable quality is characterized by comprising the following components in percentage by mass: 0.001-0.5% of astaxanthin; polyol: 2 to 20 percent; antioxidant: 0.01-1%; 0.01-10% of skin conditioner; chelating agent: 0.01-1%; thickening agent: 0.01-1%; pH regulators: 0.01-1%; 0.1-20% of grease; emulsifier: 0.01 to 5 percent; preservative: 0.05-2%; 50-80% of water.

2. The astaxanthin antioxidant essence milk with stable quality as claimed in claim 1, wherein the polyalcohol is one or more of propylene glycol, butanediol, glycerol and pentanediol.

3. The astaxanthin antioxidant essence milk with stable quality as claimed in claim 1, wherein the antioxidant is one or more of sodium metabisulfite, tocopherol and tocopherol acetate.

4. The astaxanthin antioxidant essence milk with stable quality as claimed in claim 1, wherein the skin conditioning agent is one or more of allantoin, sodium hyaluronate, sodium PCA, hydrolyzed collagen and hydrolyzed sclerotium rolfsii gum.

5. The astaxanthin antioxidant essence milk with stable quality as claimed in claim 1, wherein the chelating agent is one or more of EDTA-2Na and EDTA-4 Na;

the thickening agent is one or more of xanthan gum, crinkle-wave carrageenan, acrylic acid (ester)/C10-30 alkanol acrylate cross-linked polymer, acryloyl dimethyl taurate/VP copolymer, hydroxyethyl acrylate/acryloyl dimethyl taurate copolymer and hydroxyethyl cellulose.

6. The astaxanthin antioxidant essence milk with stable quality as claimed in claim 1, wherein the pH regulator is one or more of citric acid, sodium citrate, triethanolamine and aminomethyl propanol.

7. The astaxanthin antioxidant essence milk with stable quality as claimed in claim 1, wherein the oil is one or more of hydrogenated polyisobutene, dioctyl carbonate, isohexadecane, isononyl isononanoate, caprylic/capric triglyceride.

8. The astaxanthin antioxidant essence milk with stable quality as claimed in claim 1, wherein the emulsifier is one or more of sorbitan stearate, polysorbate-60, PEG-100 stearate and glycerol stearate.

9. The astaxanthin antioxidant essence milk with stable quality as claimed in claim 1, wherein the preservative is one or more of methyl hydroxybenzoate, propyl hydroxybenzoate, phenoxyethanol, ethylhexyl glycerol and p-hydroxyacetophenone.

10. A method for preparing astaxanthin antioxidant essence milk with stable quality according to any one of claims 1 to 9, wherein the method comprises the following steps: