CN114259454A - Tear-type Zhejiang radix ophiopogonis whitening mask and preparation method thereof - Google Patents
Tear-type Zhejiang radix ophiopogonis whitening mask and preparation method thereof Download PDFInfo
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- CN114259454A CN114259454A CN202210082635.5A CN202210082635A CN114259454A CN 114259454 A CN114259454 A CN 114259454A CN 202210082635 A CN202210082635 A CN 202210082635A CN 114259454 A CN114259454 A CN 114259454A
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- extract
- whitening
- weight
- tear
- sodium
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- 229930195210 Ophiopogon Natural products 0.000 claims abstract description 54
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- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 claims abstract description 30
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Images
Abstract
The invention discloses a tear-off type Zhejiang radix ophiopogonis whitening mask which comprises the following components in percentage by weight: 1-6% of Zhejiang ophiopogon root homoisoflavone extract, 0.04-0.4% of whitening reinforcing agent, 0.05-0.5% of absorption enhancer, 1-7% of complexing agent, 0.1-0.5% of sodium carboxymethylcellulose, 0.01-0.05% of sodium hyaluronate, 10-20% of glycerol, 2-5% of ethylene glycol, 10-30% of polyvinyl alcohol, 0.05-0.1% of tea oil, 0.78-2% of tween-800.05, 0.05-2% of azone, 0.1-0.5% of ethylparaben, 0.05-0.5% of allantoin and the balance of deionized water. The high isoflavone extract of the thunberg dwarf lilyturf tuber used in the invention can effectively inhibit tyrosinase activity and effectively reduce chloasma and black specks caused by acne, has rich sources, belongs to renewable resources and is green and environment-friendly.
Description
Technical Field
The invention belongs to the technical field of cosmetics, and particularly relates to a tear-off type Zhe radix ophiopogonis whitening mask and a preparation method thereof.
Background
The facial mask is a facial skin cosmetic which is applied on the surface of human skin and is removed, scrubbed or kept after a period of time, so that the facial skin cosmetic integrates cleaning, nursing and nutrition, and is popular among adults, especially female consumers. With the maturity of consumption psychology, people not only require that the facial mask can achieve basic effects of cleaning, nursing and nutrition, but also further pursue the development of advanced effects of whitening, anti-aging and the like of the facial mask. At present, the facial masks are various in types, and are classified into a patch facial mask, a tear facial mask, a gel facial mask and the like. The tearing mask is a sticky paste, is uniformly smeared on the face for 15-25 minutes, can form a layer of film on the face along with the volatilization of moisture, can be separated from the face in a tearing mode, and in the process, dirt, scurf and the like on the skin of the face can be adhered to the film and removed together, so that the effect of cleaning the face is achieved. Meanwhile, due to the good physical properties of the tear-off facial mask, the tear-off facial mask can be a good medicine carrier, and different medicines are added into the tear-off facial mask, so that multiple effects of cleaning and beautifying can be achieved.
The color of skin is controlled by various factors, mainly depending on the content and distribution of melanin. Melanin is an amino acid derivative formed by a series of chemical reactions, usually in the form of polymerization, of tyrosine or 3, 4-dihydroxyphenylalanine. The melanin is synthesized by melanocytes in the basal layer of human epidermis, when ultraviolet rays irradiate the skin, the skin is in a self-protection state, the activity of tyrosinase is activated, and the oxidation of tyrosine or 3, 4-dihydroxyphenylalanine is catalyzed to generate the melanin, so that the skin cells are protected. Melanin moves layer by layer through cell metabolism, and forms freckles, sunburn, black spots and the like on the skin epidermis. With the development of modernization of traditional Chinese medicines, more and more traditional Chinese medicines are found to have the effect of beautifying and are applied to skin care products. Zhejiang lilyturf root is one of the best famous genuine medicinal materials of Zhejiang province, namely Zhejiang province, and has been used for treating acute cough, sore throat, cardiovascular and cerebrovascular diseases and the like for thousands of years. In 2002, radix ophiopogonis is approved by the national Weijian Commission as a 'medicine and food homologous' traditional Chinese medicine for health-care food; in addition, it is also used as a functional food and a local medicine in southeast asian countries such as japan and vietnam. Researches show that the flavonoid component is one of the main drug-effect substances; in the previous researches, the radix ophiopogonis tuber and fibrous root contain characteristic flavonoids, including methyl radix ophiopogonis flavanone A, methyl radix ophiopogonis flavanone B, 6-aldehyde isoophiopogonis flavanone A, 6-aldehyde isoophiopogonis flavanone B and the like, which have the effect of inhibiting tyrosinase, so that the generation of melanin in cells is blocked, and therefore, the radix ophiopogonis tuber and fibrous root can be used in skin care products with the effects of whitening and the like to achieve the effects of beautifying and removing freckles. The ophiopogon root extract is used in a plurality of patents for preparing whitening masks, for example, Chinese patent CN111956543A discloses a whitening and anti-allergy cannabis leaf mask, and the traditional Chinese medicine composition consists of the following raw materials in parts by weight: 60-92% of water, 1-6% of propylene glycol, 1-6% of glycerol, 0.05-3% of cactus stem extract, 0.05-3% of radix ophiopogonis extract, 0.05-3% of radix sophorae flavescentis extract, 0.1-6% of trehalose, 0.1-6% of butanediol, 0.05-3% of snow lotus extract, 0.05-3% of leontopodium japonicum flower/leaf extract, 0.001-0.3% of tartaric acid, 0.001-0.3% of disodium EDTA, 0.001-0.3% of sodium sulfite, 0.001-0.3% of sodium metabisulfite, 0.1-2% of tremella extract, 0.1-1% of p-hydroxyacetophenone, 0.1, 2-1% of hexanediol, 0.05-0.2% of xanthan gum, 0.05-0.2% of allantoin, 0.05-5% of cannabis leaf extract and 0.05-0.2% of sodium polyacrylate. The prepared facial mask contains 0.05-3% radix Ophiopogonis extract. Chinese patent CN113041205A A whitening and moisturizing traditional Chinese medicine mask and a preparation method thereof, wherein the whitening and moisturizing traditional Chinese medicine mask is prepared by taking 10-300 parts by weight of semen cuscutae, 10-200 parts by weight of safflower, 10-100 parts by weight of tribulus terrestris, 1-50 parts by weight of radix ophiopogonis, 50-500 parts by weight of leek leaves, 5-50 parts by weight of loess, 10-100 parts by weight of vegetable oil and 1000 parts by weight of starch as raw materials through the steps of crushing, ultrasonic extraction, pH adjustment and the like. Although the formula of the facial mask preparation method contains the radix ophiopogonis extract, the radix ophiopogonis is not taken as a main drug in the formula composition, and the structure type and the content standard of the effective components of the radix ophiopogonis in the facial mask are not clear. Therefore, based on the existing research and experiment results, the traditional Chinese medicine mask containing the high isoflavone component extract of the Zhejiang ophiopogon root has good whitening efficacy and market potential.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a tear-off type Zhe radix ophiopogonis whitening mask and a preparation method thereof, and the tear-off type Zhe radix ophiopogonis whitening mask is realized by the following technical scheme:
the tearing type Zhejiang radix ophiopogonis whitening mask comprises the following components in percentage by weight:
1-6% of Zhejiang ophiopogon root homoisoflavone extract, 0.04-0.4% of whitening reinforcing agent, 0.05-0.5% of absorption enhancer, 1-7% of complexing agent, 0.1-0.5% of sodium carboxymethylcellulose, 0.01-0.05% of sodium hyaluronate, 10-20% of glycerol, 2-5% of ethylene glycol, 10-30% of polyvinyl alcohol, 0.05-0.1% of tea oil, 0.78-2% of tween-800.05, 0.05-2% of azone, 0.1-0.5% of ethylparaben, 0.05-0.5% of allantoin and the balance of deionized water.
Further, the paint comprises the following components in percentage by weight:
5% of Zhejiang ophiopogon root homoisoflavone extract, 0.3% of whitening reinforcing agent, 0.48% of absorption enhancer, 2% of complexing agent, 0.2% of sodium carboxymethylcellulose, 0.04% of sodium hyaluronate, 20% of glycerol, 5% of ethylene glycol, 25% of polyvinyl alcohol, 0.05% of tea oil, tween-800.05%, 1.5% of azone, 0.3% of ethylparaben, 0.1% of allantoin and the balance of deionized water.
Further, the complexing agent is one or two of EDTA-disodium or chitosan, the weight percentage of the EDTA-disodium is 2-3%, and the weight percentage of the chitosan is 1-4%.
Furthermore, the Zhejiang ophiopogon root isoflavone extract means that the total content of the methyl ophiopogonone A, the methyl ophiopogonone B, the 6-aldehyde isoophiopogonone A and the 6-aldehyde isoophiopogonone B in the Zhejiang ophiopogon root isoflavone extract is not less than 10 percent according to dry products.
Further, the whitening enhancer is one or two of vitamin B1 and vitamin C.
Further, the absorption enhancer is composed of steroidal saponins of Thunberg ophiopogon root and cholate; the mass ratio of the steroidal saponins of the Thunberg ophiopogon root to the cholate is 3:1, and the total saponins of the Thunberg ophiopogon root calculated by ruscogenin in the dry product is not less than 5%; the cholate is selected from one or more of sodium glycocholate, sodium glycochenodeoxycholate, sodium taurocholate, sodium taurochenodeoxycholate and sodium deoxycholate.
Furthermore, the tea oil is cold-pressed camellia oil, the camellia oil is comparable to olive oil, and the fatty acid composition is similar to that of the olive oil. The preparation method comprises the following steps:
selecting ripe camellia seeds, drying at 40-50 ℃ until the water content is 3-6%, and conveying the dried camellia seeds into a huller for hulling; cold pressing the shelled camellia seeds to obtain camellia oil, wherein the temperature of a press chamber is 100-150 ℃, and the oil outlet temperature is 80-120 ℃; removing solid impurities from the pressed camellia oil by a plate-and-frame filter press; winterizing the camellia oil subjected to plate-and-frame filter pressing at-5 ℃; removing free fatty acid, lipid peroxidation products, water and other low boiling point substances in the winterized camellia oil by molecular distillation; filtering the camellia oil subjected to molecular distillation by using a mixture of argil, activated carbon and alumina as a filter medium to remove impurities and pigments to obtain a finished product.
Further, the Zhejiang ophiopogon root homoisoflavone extract is prepared by the following method:
1) adding 20 times of 70% ethanol into the powder of radix Ophiopogonis, reflux-extracting at 80 deg.C for 2 hr, concentrating the filtrate to obtain extract, and diluting with deionized water to obtain water extract with concentration of 0.1-1g per 1 ml;
2) taking the extract obtained in the step 1), adding 0.5-2 times volume ratio of water saturated ethyl acetate for extraction, extracting for 2-5 times to obtain ethyl acetate extract, concentrating under reduced pressure, and freeze-drying under vacuum to obtain extract, namely the total homoisoflavone extract of the Zhejiang ophiopogon root; extracting the residual water solution, continuously adding water saturated n-butanol with volume ratio of 0.5-2 times, extracting for 2-5 times to obtain n-butanol extractive solution, concentrating under reduced pressure, and vacuum freeze drying to obtain extract, i.e. steroid saponin extract of radix Ophiopogonis.
The preparation method of the tear-off type Zhejiang radix ophiopogonis whitening mask is prepared by the following steps:
1) taking sodium carboxymethylcellulose and polyvinyl alcohol according to the formula amount, adding a proper amount of deionized water, heating and stirring at 70-90 ℃ to fully dissolve the sodium carboxymethylcellulose and the polyvinyl alcohol, adding allantoin and sodium hyaluronate according to the formula amount after the sodium carboxymethylcellulose and the polyvinyl alcohol are uniformly dispersed, continuously heating and stirring to 80 ℃, uniformly cooling to room temperature to obtain paste A;
2) taking the formula amount of glycerol, ethylene glycol, methyl paraben, the high isoflavone extract of the thunberg dwarf lilyturf tuber, tea oil, an absorption enhancer, tween-80, azone and a whitening enhancer, adding a proper amount of deionized water, stirring uniformly at 40-50 ℃, and dissolving by ultrasonic waves to obtain a liquid B;
3) placing the paste A and the liquid B in a vacuum homogenizer, adding deionized water to make up the balance, stirring uniformly in vacuum, and packaging to obtain the final product.
Further, a proper amount of deionized water in the step 1) accounts for 70-80% of the total amount of the deionized water, and a complexing agent is also added in the step 1), wherein the complexing agent is one or two of EDTA-disodium and chitosan.
The tear type Zhe radix ophiopogonis whitening mask is applied to relieving chloasma and black spots caused by acne.
Compared with the prior art, the invention has the following beneficial effects:
1) the high isoflavone extract of the Zhejiang dwarf lilyturf tuber used in the invention can effectively inhibit the activity of tyrosinase and effectively reduce chloasma and black specks caused by acne. And the extract has clear functional components, exact effect and clear allergen screening. The high isoflavone extract of the thunberg dwarf lilyturf tuber is prepared by extracting natural plant thunberg dwarf lilyturf tuber, has rich sources, belongs to renewable resources and is green and environment-friendly;
2) in the formula, the high isoflavone extract of the Zhejiang ophiopogon root is used as a functional factor, and the steroid saponin extract of the Zhejiang ophiopogon root is used as a natural nonionic surfactant, so that the high-efficiency comprehensive utilization of the Zhejiang ophiopogon root resource is realized, tiny colloid particles can be formed in water by using the structural characteristics of the saponin, active ingredients in the formula are adsorbed together by forming micelle action, the permeability of intercellular water-soluble channels is increased, and the absorption of water-soluble substances is promoted; the low-concentration cholate can hydrate and extract intercellular lipid, so that the diffusion of the extract in intercellular aqueous channels is increased, the cholate can be used as an enzyme inhibitor, the stability of the medicament is maintained by influencing the activity of the enzyme and changing different mechanisms such as polypeptide and protein conformation, and the absorption of active ingredients in the whitening mask can be obviously increased by compounding the cholate with the steroid saponin extract of the surfactant Zhe ophiopogon japonicus;
3) all components in the formula are nontoxic, non-irritant and high in safety performance, most of the components are natural plant extracted active ingredients, and the components can be used safely.
Drawings
FIG. 1 is a HPLC chromatogram for measuring homoisoflavone flavone standard;
FIG. 2 is HPLC chromatogram for measuring the content of homoisoflavone in the homoisoflavone extract of Thunberg dwarf lilyturf tuber;
in the figure, 1 is methyl ophiopogon root flavanone A; 2 is radix Ophiopogonis flavanone B; 3 is 6-aldehyde isoophiopogonone flavanone A; 4 is 6-aldehyde isoophiopogonone B.
Detailed Description
The present invention will be further described with reference to specific examples in order to better understand the present technical solution. In the following examples, the percentages referred to are by weight unless otherwise indicated.
Example 1
3% of Zhejiang ophiopogon root homoisoflavone extract, 0.2% of vitamin C, 0.3% of Zhejiang ophiopogon root steroid saponin extract, 0.1% of sodium glycocholate, 0.3% of sodium carboxymethylcellulose, 0.03% of sodium hyaluronate, 10% of glycerol, 2% of ethylene glycol, 20% of polyvinyl alcohol, 0.1% of tea oil, tween-801%, 1% of azone, 0.2% of ethylparaben, 0.2% of allantoin, 2% of chitosan and the balance of deionized water.
The preparation method comprises the following steps:
1) taking 0.3 weight part of sodium carboxymethylcellulose and 20 weight parts of polyvinyl alcohol, adding 45 weight parts of deionized water, heating and stirring at 70-90 ℃ to fully dissolve the sodium carboxymethylcellulose and the polyvinyl alcohol, adding 0.2 weight part of allantoin, 0.03 weight part of sodium hyaluronate and 2 weight parts of chitosan after the mixture is uniformly dispersed, continuously heating and stirring to 80 ℃, and cooling to room temperature to obtain paste A after the mixture is uniformly dispersed;
2) taking 10 parts by weight of glycerol, 2 parts by weight of ethylene glycol, 0.2 part by weight of methylparaben, 3 parts by weight of Zhejiang ophiopogon root homoisoflavonoid extract, 0.1 part by weight of tea oil, 0.3 part by weight of Zhejiang ophiopogon root steroid saponin extract, 0.1 part by weight of sodium glycocholate, 1 part by weight of Tween-80, 1 part by weight of azone, 0.2 part by weight of vitamin C and adding a proper amount of deionized water, stirring uniformly at 40-50 ℃, and dissolving by ultrasonic waves to obtain a liquid B;
3) placing the paste A and the liquid B in a vacuum homogenizer, adding deionized water to make up the balance, stirring uniformly in vacuum, and packaging to obtain the final product.
Example 2
5% of Zhejiang ophiopogon root homoisoflavone extract, 0.3% of vitamin C, 0.36% of Zhejiang ophiopogon root steroid saponin extract, 0.12% of sodium glycocholate, 0.2% of sodium carboxymethylcellulose, 0.04% of sodium hyaluronate, 20% of glycerol, 5% of glycol, 25% of polyvinyl alcohol, 0.05% of tea oil, 1.5% of tween-800.05% of azone, 0.3% of ethylparaben, 0.1% of allantoin, 3% of EDTA-disodium and the balance of deionized water.
The preparation method comprises the following steps:
1) taking 0.2 part by weight of sodium carboxymethylcellulose and 25 parts by weight of polyvinyl alcohol, adding 30 parts by weight of deionized water, heating and stirring at 70-90 ℃ to fully dissolve the sodium carboxymethylcellulose and the polyvinyl alcohol, adding 0.1 part by weight of allantoin, 0.04 part by weight of sodium hyaluronate and 3 parts by weight of EDTA-disodium after the sodium carboxymethylcellulose and the polyvinyl alcohol are uniformly dispersed, continuously heating and stirring to 80 ℃, and cooling to room temperature to obtain paste A;
2) taking 20 parts by weight of glycerol, 5 parts by weight of ethylene glycol, 0.3 part by weight of methylparaben, 5 parts by weight of Zhejiang ophiopogon root homoisoflavonoid extract, 0.05 part by weight of tea oil, 0.36 part by weight of Zhejiang ophiopogon root steroid saponin, 0.12 part by weight of sodium glycocholate, 0.05 part by weight of Tween-80, 1.5 parts by weight of azone and 0.3 part by weight of vitamin C, adding a proper amount of deionized water, uniformly stirring at 40-50 ℃, and dissolving by ultrasonic waves to obtain a liquid B;
3) placing the paste A and the liquid B in a vacuum homogenizer, adding deionized water to make up the balance, stirring uniformly in vacuum, and packaging to obtain the final product.
Example 3
1% of Zhejiang ophiopogon root homoisoflavone extract, 10.3% of vitamin B, 0.21% of Zhejiang ophiopogon root steroid saponin extract, 0.07% of sodium glycocholate, 0.5% of sodium carboxymethylcellulose, 0.05% of sodium hyaluronate, 15% of glycerol, 4% of ethylene glycol, 15% of polyvinyl alcohol, 0.05% of tea oil, tween-800.05%, 2% of azone, 0.5% of ethylparaben, 0.4% of allantoin, 2% of EDTA-disodium and the balance of deionized water.
The preparation method comprises the following steps:
1) taking 0.5 weight part of sodium carboxymethylcellulose and 15 weight parts of polyvinyl alcohol, adding 45 weight parts of deionized water, heating and stirring at 70-90 ℃ to fully dissolve the sodium carboxymethylcellulose and the polyvinyl alcohol, adding 0.4 weight part of allantoin, 0.05 weight part of sodium hyaluronate and 2 weight parts of EDTA-disodium after the sodium carboxymethylcellulose and the polyvinyl alcohol are uniformly dispersed, continuously heating and stirring to 80 ℃, and cooling to room temperature to obtain paste A;
2) taking 15 parts by weight of glycerol, 4 parts by weight of ethylene glycol, 0.5 part by weight of methylparaben, 1 part by weight of ophiopogonin extract, 0.05 part by weight of tea oil, 0.2 part by weight of Zhejiang ophiopogonin steroid saponin, 0.06 part by weight of sodium glycocholate, 0.05 part by weight of tween-80, 2 parts by weight of azone and 0.3 part by weight of vitamin B1, adding a proper amount of deionized water, stirring uniformly at 40-50 ℃, and dissolving by ultrasonic waves to obtain liquid B;
3) placing the paste A and the liquid B in a vacuum homogenizer, adding deionized water to make up the balance, stirring uniformly in vacuum, and packaging to obtain the final product.
Example 4
6% of Zhejiang ophiopogon root homoisoflavonoid extract, 10.2% of vitamin B, 0.3% of Zhejiang ophiopogon root steroid saponin extract, 0.1% of sodium glycocholate, 0.1% of sodium carboxymethylcellulose, 0.01% of sodium hyaluronate, 20% of glycerol, 3% of ethylene glycol, 10% of polyvinyl alcohol, 0.05% of tea oil, tween-800.1%, 0.2% of azone, 0.1% of ethylparaben, 0.3% of allantoin, 4% of chitosan and the balance of deionized water.
The preparation method comprises the following steps:
1) taking 0.1 part by weight of sodium carboxymethylcellulose and 10 parts by weight of polyvinyl alcohol, adding 40 parts by weight of deionized water, heating and stirring at 70-90 ℃ to fully dissolve the sodium carboxymethylcellulose and the polyvinyl alcohol, adding 0.3 part by weight of allantoin, 0.01 part by weight of sodium hyaluronate and 4 parts by weight of chitosan after the sodium carboxymethylcellulose and the polyvinyl alcohol are uniformly dispersed, continuously heating and stirring to 80 ℃, and cooling to room temperature to obtain paste A;
2) taking 20 parts by weight of glycerol, 1 part by weight of ethylene glycol, 0.1 part by weight of methylparaben, 6 parts by weight of ophiopogonin extract, 0.05 part by weight of tea oil, 0.3 part by weight of Zhejiang ophiopogonin steroid saponin extract, 0.1 part by weight of sodium glycocholate, 0.1 part by weight of Tween-80, 0.05 part by weight of azone and 0.2 part by weight of vitamin B1, adding a proper amount of deionized water, stirring uniformly at 40-50 ℃, and dissolving by ultrasonic waves to obtain liquid B;
3) placing the paste A and the liquid B in a vacuum homogenizer, adding deionized water to make up the balance, stirring uniformly in vacuum, and packaging to obtain the final product.
Example 5
3% of Zhejiang ophiopogon root homoisoflavone extract, 10.2% of vitamin B, 0.2% of vitamin C, 0.3% of Zhejiang ophiopogon root steroid saponin extract, 0.1% of sodium glycocholate, 0.2% of sodium carboxymethylcellulose, 0.02% of sodium hyaluronate, 18% of glycerol, 3% of ethylene glycol, 10% of polyvinyl alcohol, 0.05% of tea oil, 800.1% of tween-1, 0.05% of azone, 0.4% of ethylparaben, 0.5% of allantoin, 1% of chitosan and the balance of deionized water.
The preparation method comprises the following steps:
1) taking 0.2 part by weight of sodium carboxymethylcellulose and 10 parts by weight of polyvinyl alcohol, adding 48 parts by weight of deionized water, heating and stirring at 70-90 ℃ to fully dissolve the sodium carboxymethylcellulose and the polyvinyl alcohol, adding 0.5 part by weight of allantoin and 0.02 part by weight of sodium hyaluronate after the sodium carboxymethylcellulose and the polyvinyl alcohol are uniformly dispersed, continuing heating and stirring to 80 ℃, and cooling to room temperature to obtain paste A after the sodium hyaluronate and the allantoin are uniformly dispersed;
2) taking 18 parts by weight of glycerol, 3 parts by weight of ethylene glycol, 0.4 part by weight of methylparaben, 3 parts by weight of ophiopogonin extract, 0.05 part by weight of tea oil, 0.3 part by weight of Zhejiang ophiopogonin steroid saponin extract, 0.1 part by weight of sodium glycocholate, 0.1 part by weight of Tween-80, 0.05 part by weight of azone, 0.2 part by weight of vitamin C and 0.2 part by weight of vitamin B1, adding a proper amount of deionized water, stirring uniformly at 40-50 ℃, and dissolving by ultrasonic waves to obtain liquid B;
3) placing the paste A and the liquid B in a vacuum homogenizer, adding deionized water to make up the balance, stirring uniformly in vacuum, and packaging to obtain the final product.
Examples of the experiments
Experimental example 1: analysis of four homoisoflavonoids in the homoisoflavonoids from Thunberg dwarf lilyturf root extract the HPLC conditions used in this example for analyzing the homoisoflavonoids from Thunberg dwarf lilyturf root extract and products were as follows: the Waters HPLC system comprised an e2695 quaternary pump separation unit, column oven and 2998 diode array detector; column Thermo C18 column (4.6X 250mm,5.0 μm); the mobile phase consists of acetonitrile (A) and water (B), and the gradient elution scheme is as follows: 0-5min, 35% A; 5-20min, 35-40% A; 20-50min, 40-70% A. The column temperature is 35 ℃; the flow rate was 1mL/min, and the detection wavelength was 285 nm. The amount of the sample is generally 5 to 20. mu.L depending on the concentration of the sample. HPLC detection spectra of 4 kinds of radix Ophiopogonis homoisoflavone standard and sample are shown in FIGS. 1 and 2.
Experimental example 2: tyrosinase inhibitory activity research of high isoflavone extract of Zhejiang ophiopogon root
Phosphate (p H6.8.8, 0.05mol/L) buffer configuration:
preparation of tyrosinase solution: weighing tyrosinase precisely, and preparing into 5 × 10 with sodium phosphate buffer solution-6The enzyme solution of mol/L is frozen and preserved at minus 20 ℃ and unfrozen at the previous 4 ℃.
Preparing an L-DOPA (L-DOPA) solution: precisely weighing L-DOPA, adding phosphate buffer solution for dissolving to obtain 5.0 × 10-4A mol/L-dopa solution.
Preparation of sample solution: preparing homoisoflavone compound solutions with different concentrations from the homoisoflavone extract of Thunberg dwarf lilyturf root.
The determination method comprises the following steps: the product generated by catalyzing substrate L-DOPA with tyrosinase has a characteristic absorption peak at 475nm, and the concentration of tyrosinase is fixed to be 2.08 multiplied by 10 in a 3mL phosphate (pH 6.8, 0.05mol/L) buffer system by utilizing an inhibition kinetic method-7mol/L, incubating with homoisoflavone extracts of different concentrations at room temperature for 3 hr for full reaction, adding L-DOPA (5.0 × 10) as substrate-4mol/L) of the obtained product, measuring the absorbance of the reaction system at 475nm every 5s, and calculating tyrosinase in the systems containing different concentrations of homoisoflavone according to the relation (1)Relative activity of (2). Kojic acid was used as a positive control. Wherein R0 and R are respectively the change rate of the absorbance of the reaction system with time when no inhibitor is added and different concentrations of the inhibitor are added. The results of the activity inhibition are shown in Table 1.
Relative activity (%) - (R/R0). times.100% (1)
TABLE 1 tyrosinase activity inhibition rate of high isoflavone extract from Thunberg lilyturf root
Experimental results show that the high isoflavone extract of the Zhejiang ophiopogon root has obvious tyrosinase activity inhibition effect. The invention can effectively reduce chloasma and black spots caused by acne, and has the functions of removing freckles, whitening and moisturizing.
Experimental example 3: research on inhibitory activity of polysaccharide and water extract tyrosinase of Zhejiang ophiopogon root
The tyrosinase inhibitory activity of polysaccharide and aqueous extracts of radix Ophiopogonis with different concentrations was determined by the same method as in Experimental example 2, and the results are shown in Table 2.
TABLE 2 tyrosinase activity inhibition rate of polysaccharide and water extract of Zhejiang ophiopogon root
Experimental results show that compared with the high isoflavone extract of the Zhejiang ophiopogon root, the Zhejiang ophiopogon root polysaccharide and the water extract have lower inhibition rate on tyrosinase activity and have no obvious inhibition effect on tyrosinase at each concentration, which indicates that the Zhejiang ophiopogon root polysaccharide and the water extract are not effective components for whitening the Zhejiang ophiopogon root.
Experimental example 4: research on tyrosinase activity inhibition by synergism of high isoflavone extract of Thunberg ophiopogon root and whitening enhancer
The whitening and strengthening compound liquid is prepared by the Zhejiang ophiopogon root homoisoflavone extract and the strengthening agents with different proportions. The Zhe ophiopogon root homoisoflavone extract and whitening enhancer complex solution prepared according to the example 1 is marked as complex solution 1, the ophiopogon root homoisoflavone extract and whitening enhancer complex solution prepared according to the example 2 is marked as complex solution 2, and so on. The inhibitory activity of the complex solution and the homoisoflavonoid extract of Zhejiang ophiopogon root on tyrosinase was determined by the same method as in Experimental example 1, and the concentration of the homoisoflavonoid extract of Zhejiang ophiopogon root was 100% (calculated based on crude drug), and the results are shown in Table 3.
TABLE 3 tyrosinase activity inhibition rate for each sample
Experimental example 5: basic physical and chemical indexes
The color, smell, spreadability, viscosity, product structure and stability of the facial mask are tested according to national standards QB/T1857-2013 and QB/T2660-2004 to determine whether the facial mask meets the national standards. The related physicochemical detection indexes, sensory and stability test results of the mask sample are shown in table 4.
TABLE 4 physicochemical index, sensory and stability test results
Experimental example 6 skin irritation test
30 volunteers aged 20-30 years were selected as the test subjects, and the mask was applied evenly to the back of their left hand 2 times a day, and the skin reaction was observed after 6 hours. Through experimental observation of a week, the back skin of the left hand coated with the facial mask solution of 30 healthy college student volunteers is softer and more moist than the back skin of the right hand without the facial mask solution, and the phenomena of redness, eruption, blister and the like are not seen, and the phenomena of itching, allergy, pain and the like are also avoided, so that the facial mask is free of irritation.
Claims (10)
1. The tear-off type Zhe radix ophiopogonis whitening mask is characterized by comprising the following components in percentage by weight:
1-6% of Zhejiang ophiopogon root homoisoflavone extract, 0.04-0.4% of whitening reinforcing agent, 0.05-0.5% of absorption enhancer, 1-7% of complexing agent, 0.1-0.5% of sodium carboxymethylcellulose, 0.01-0.05% of sodium hyaluronate, 10-20% of glycerol, 2-5% of ethylene glycol, 10-30% of polyvinyl alcohol, 0.05-0.1% of tea oil, 0.78-2% of tween-800.05, 0.05-2% of azone, 0.1-0.5% of ethylparaben, 0.05-0.5% of allantoin and the balance of deionized water.
2. The tear-off type Thunberg tuber whitening mask as claimed in claim 1 or 3, which is characterized by comprising the following components in percentage by weight:
5% of Zhejiang ophiopogon root homoisoflavone extract, 0.3% of whitening reinforcing agent, 0.48% of absorption enhancer, 3% of complexing agent, 0.2% of sodium carboxymethylcellulose, 0.04% of sodium hyaluronate, 20% of glycerol, 5% of ethylene glycol, 25% of polyvinyl alcohol, 0.05% of tea oil, tween-800.05, 1.5% of azone, 0.3% of ethylparaben, 0.1% of allantoin and the balance of deionized water.
3. The tear-off type Thunberg dwarf lilyturf whitening mask as claimed in claim 1, wherein the complexing agent is one or two of EDTA-disodium or chitosan, the weight percentage of EDTA-disodium is 2-3%, and the weight percentage of chitosan is 1-4%.
4. The tear-off type Zhe ophiopogon whitening mask as claimed in claim 1 or 2, wherein the Zhe ophiopogon japonicus isoflavone extract contains not less than 10% of the total amount of methyl ophiopogonone A, methyl ophiopogonone B, 6-aldehydio ophiopogonone A and 6-aldehydio ophiopogonone B in terms of dry product.
5. The tear-off type Thunberg dwarf lilyturf whitening mask as claimed in claim 1 or 2, wherein the whitening enhancer is one or both of vitamin B1 and vitamin C.
6. The tear-off type Zhe ophiopogon whitening mask as claimed in claim 1 or 2, wherein said absorption enhancer is composed of steroidal saponins of Zhe ophiopogon and cholate; the mass ratio of the steroidal saponins of the Thunberg ophiopogon root to the cholate is 3:1, and the total saponins of the Thunberg ophiopogon root calculated by ruscogenin in the dry product is not less than 5%; the cholate is selected from one or more of sodium glycocholate, sodium glycochenodeoxycholate, sodium taurocholate, sodium taurochenodeoxycholate and sodium deoxycholate.
7. The tear-off type Zhe ophiopogon whitening mask as claimed in claim 1 or 2, wherein the Zhe ophiopogon japonicus homoisoflavone extract is prepared by the following method:
1) adding 20 times of 70% ethanol into the powder of radix Ophiopogonis, reflux-extracting at 80 deg.C for 2 hr, concentrating the filtrate to obtain extract, and diluting with deionized water to obtain water extract with concentration of 0.1-1g per 1 ml;
2) taking the extract obtained in the step 1), adding 0.5-2 times volume ratio of water saturated ethyl acetate for extraction, extracting for 2-5 times to obtain ethyl acetate extract, concentrating under reduced pressure, and freeze-drying under vacuum to obtain extract, namely the total homoisoflavone extract of the Zhejiang ophiopogon root; extracting the residual water solution, continuously adding water saturated n-butanol with volume ratio of 0.5-2 times, extracting for 2-5 times to obtain n-butanol extractive solution, concentrating under reduced pressure, and vacuum freeze drying to obtain extract, i.e. steroid saponin extract of radix Ophiopogonis.
8. The preparation method of the tear-off type Zhe ophiopogon whitening mask as claimed in claims 1-2, is characterized by comprising the following steps:
1) taking sodium carboxymethylcellulose and polyvinyl alcohol according to the formula amount, adding a proper amount of deionized water, heating and stirring at 70-90 ℃ to fully dissolve the sodium carboxymethylcellulose and the polyvinyl alcohol, adding allantoin and sodium hyaluronate according to the formula amount after the sodium carboxymethylcellulose and the polyvinyl alcohol are uniformly dispersed, continuously heating and stirring to 80 ℃, uniformly cooling to room temperature to obtain paste A;
2) taking the formula amount of glycerol, ethylene glycol, methyl paraben, the high isoflavone extract of the thunberg dwarf lilyturf tuber, tea oil, an absorption enhancer, tween-80, azone and a whitening enhancer, adding a proper amount of deionized water, stirring uniformly at 40-50 ℃, and dissolving by ultrasonic waves to obtain a liquid B;
3) placing the paste A and the liquid B in a vacuum homogenizer, adding deionized water to make up the balance, stirring uniformly in vacuum, and packaging to obtain the final product.
9. The preparation method of the tear-off type Thunberg radix Ophiopogonis whitening mask as claimed in claim 8, wherein an amount of deionized water in step 1) is 70-80% of the total amount of deionized water, and a complexing agent is further added in step 1), wherein the complexing agent is one or both of EDTA-disodium and chitosan.
10. Application of tear-off type Zhe radix Ophiopogonis whitening facial mask in relieving chloasma and black speck caused by acne is provided.
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