CN113876624A - Facial mask essence containing hyaluronic acid and preparation method thereof - Google Patents
Facial mask essence containing hyaluronic acid and preparation method thereof Download PDFInfo
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- CN113876624A CN113876624A CN202111182105.XA CN202111182105A CN113876624A CN 113876624 A CN113876624 A CN 113876624A CN 202111182105 A CN202111182105 A CN 202111182105A CN 113876624 A CN113876624 A CN 113876624A
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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
- A61K8/72—Cosmetics or similar toiletry preparations characterised by the composition containing organic macromolecular compounds
- A61K8/73—Polysaccharides
- A61K8/735—Mucopolysaccharides, e.g. hyaluronic acid; Derivatives thereof
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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
- A61K8/40—Cosmetics or similar toiletry preparations characterised by the composition containing organic compounds containing nitrogen
- A61K8/44—Aminocarboxylic acids or derivatives thereof, e.g. aminocarboxylic acids containing sulfur; Salts; Esters or N-acylated derivatives thereof
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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
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
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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
- A61K8/64—Proteins; Peptides; Derivatives or degradation products thereof
- A61K8/645—Proteins of vegetable origin; Derivatives or degradation products thereof
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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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Abstract
The invention relates to a facial mask, in particular to facial mask essence containing hyaluronic acid and a preparation method thereof. A facial mask essence containing hyaluronic acid comprises water, reduced glutathione, hyaluronic acid, other adjuvants and plant antibacterial peptide with cation. The reduced glutathione has high bioavailability.
Description
Technical Field
The invention relates to a facial mask, in particular to facial mask essence containing hyaluronic acid and a preparation method thereof.
Background
The facial mask is a daily skin care product, when the facial mask covers the face, the face is temporarily isolated from air, the skin temperature is raised, the blood circulation and metabolism are accelerated, pores are expanded, the oxygen content of the skin is increased, and the facial mask is favorable for removing grease and metabolic wastes accumulated in epidermal cells. Meanwhile, moisture permeates into the horny layer of the epidermis from the mask, and the skin becomes soft, bright and elastic. The facial mask has various types, wherein the patch type facial mask consists of facial mask base cloth and essence, the base cloth is non-woven cloth simulating the human face character, and the essence contains moisture-keeping active ingredients, various auxiliary materials and the like.
Reduced Glutathione (GSH) is a tripeptide containing gamma-amide bond and sulfhydryl group, and is composed of glutamic acid, cysteine and glycine. GSH exists in each cell of organism, and the sulfhydryl group on cysteine can combine with certain drugs and toxins (such as free radical, mustard gas and various heavy metals such as plumbum, mercury and arsenic) to play a role in detoxification; GSH can also help human body to maintain normal immune system function; and due to the antioxidant capacity, the whitening, freckle removing and antiallergic effects are also applied to cosmetics. However, GSH has a good water solubility (50mg/mL), a low oil-water distribution coefficient (lgP-0.87), and is difficult to permeate the stratum corneum of the skin, and thus, studies in the field of transdermal drug delivery have been relatively rare. Furthermore, most studies on transdermal drug delivery focus more on insoluble drugs or active ingredients, and how to adopt a new formulation or a new dosage form to promote transdermal absorption thereof is rarely reported for the case of storing drugs in different layers of the skin.
It HAs been shown that low relative molecular mass (especially thousands of relative molecular mass) HA penetrates the skin more easily than high relative molecular mass HA. Therefore, the low relative molecular mass HA enters the skin more than the high relative molecular mass HA, and HAs more obvious effect on the protein and lipid of the stratum corneum, thereby showing better transdermal promotion or storage capacity of the medicine. The GSH and the HA have strong interaction, so that the transdermal absorption of the GSH can be better promoted, wherein the HA with low relative molecular mass HAs better medicament storage effect on stratum corneum and dermis, and the HA with high relative molecular mass can prevent the GSH from rapidly entering the skin. In addition, due to the limitations of raw materials, extraction processes and the like, commercial products of hyaluronic acid are not usually single molecular weight, but are mixtures of hyaluronic acid with various molecular weights and sizes.
Skin care products generally contain rich nutrient substances, microbial pollution is easily caused, and the addition of the preservative is a main means for preventing the microbial pollution of the skin care products. Among the preservatives which are frequently used and frequently used are phenoxyethanol, methylparaben, propylparaben, potassium sorbate and the like, which are all chemical preservatives, have certain irritation and toxicity, and are applied to skin care products to cause the risk of contact dermatitis and the hidden danger of residue. Therefore, the antibacterial peptide as a natural source is expected to be an urgent substitute. The plant antibacterial peptide is a polypeptide consisting of 20-60 amino acid residues, has the molecular weight of 2-7 ku, is mainly positively charged, has the charge amount of + 2- +9, and has the main biological activities of resisting bacteria, fungi, viruses, parasites and cancers. The thionine and the plant defensin in the plant antibacterial peptide are both provided with strong cations and can generate electrostatic interaction with hyaluronic acid with negative charges to separate out precipitates, and the hyaluronic acid with high molecular weight is faster than HA with low molecular weight and is easy to precipitate with the plant antibacterial peptide.
Disclosure of Invention
The invention aims to provide a mask essence containing hyaluronic acid, wherein the hyaluronic acid enhances the transdermal absorption performance of reduced glutathione, plant antibacterial peptide with strong cations is adopted to improve the antibacterial and antiseptic performance of the essence and simultaneously separate out hyaluronic acid precipitate with high molecular weight, most of hyaluronic acid with low molecular weight is separated out through pentasodium pentetate with reasonable proportion, the hyaluronic acid precipitate with high molecular weight is removed, and the bioavailability of the reduced glutathione is improved.
The purpose of the invention is realized by the following technical scheme:
a facial mask essence containing hyaluronic acid comprises water, reduced glutathione, hyaluronic acid and other adjuvants, and also comprises antibacterial peptide with cation.
Preferably, the cationic plant antimicrobial peptide is a plant defensin.
Preferably, a chelating agent is further included. Further, the chelating agent is pentasodium pentetate.
Preferably, the components of the essence are as follows: 0.1 to 0.8 percent of reduced glutathione, 0.2 to 1 percent of hyaluronic acid, 0.05 to 0.15 percent of chelating agent, 0.1 to 1 percent of plant antibacterial peptide with cations, 21 to 26 percent of other auxiliary materials and the balance of water. Other auxiliary materials include: surfactant, thickener, humectant, acidity regulator and essence.
Preferably, the components of the essence are as follows: 0.25% of reduced glutathione, 0.5% of hyaluronic acid, 0.1% of chelating agent, 0.3% of plant antibacterial peptide with cations, 25.35% of other auxiliary materials and the balance of water.
Preferably, the mass ratio of the hyaluronic acid to the plant defensin to the pentetate is 5: 3: 1.
the invention has the following effects: hyaluronic acid enhances the transdermal absorption of reduced glutathione, hyaluronic acid with low relative molecular mass can promote the transdermal absorption of glutathione, and hyaluronic acid with high molecular weight is the opposite. Because hyaluronic acid is generally a mixture with different molecular weights, in order to remove high molecular weight hyaluronic acid, plant antibacterial peptide plant defensin with cations is added, so that the high molecular weight hyaluronic acid precipitate can be preferentially separated out while the antiseptic property is improved, but a part of low molecular weight hyaluronic acid precipitate can be separated out at the same time. Part of the low molecular weight HA precipitate is resolved by adding pentasodium penta-pentetate so as to improve the content of the low molecular weight hyaluronic acid in the essence. In conclusion, the reduced glutathione provided by the invention has high bioavailability.
Drawings
FIG. 1: a standard curve graph of GSH content detection;
FIG. 2: cumulative transdermal absorption of GSH results.
Detailed Description
The present invention will be described in further detail with reference to examples.
The main raw materials and reagents used in the examples were as follows:
the reduced glutathione, the hyaluronic acid and other auxiliary materials are all commercial products, and the plant defensins are as follows: ruixin baiao biotechnology (shenzhen) ltd, pentetate: yaji Biotech, Inc., Shanghai. Bacteria and fungi: shanghai Industrial microbiology institute, wherein bacteria include: escherichia coli, Staphylococcus aureus, Bacillus megaterium, Pseudomonas aeruginosa; the fungi include Candida albicans and Aspergillus niger.
Example 1 facial mask essence preparation
Taking a facial mask essence sample 5 as an example, the preparation method comprises the following steps: adding 73.5% of deionized water, 0.25% of reduced glutathione, 0.5% of hyaluronic acid, 0.3% of phytoalexin, 0.1% of pentasodium pentetate and the rest of other auxiliary materials into a beaker in sequence, fully stirring, heating to 50-55 ℃, keeping for 15min, and cooling to below 45 ℃.
Wherein, the other auxiliary materials comprise a surfactant, a thickening agent, a humectant, an acidity regulator and essence, and account for 25.35 percent of the essence by mass.
The preparation methods of the other samples of the facial mask essence are the same and only have different formulas, and the formulas of all the samples are shown in the following table 1:
table 1 facial mask essence sample formula table
Note: "-" indicates that no material was added; wherein, the plant defensin or the essence of the thionine added in the test process is precipitated, and the plant defensin and the thionine are both provided with strong cations, hyaluronic acid is negatively charged, and the hyaluronic acid and the thionine generate electrostatic interaction.
Example 2 precipitation Rate and HA molecular weight distribution measurements
The essence samples prepared according to the formula of example 1 are respectively weighed by 10g and then centrifugally precipitated, the precipitates are taken out, the mass A of the precipitates is weighed after drying, the precipitation rate of the samples is calculated by a formula,
each sample was subjected to 3 replicates and averaged.
TABLE 2 deposition rates of essences of different formula compositions
From the experimental data in table 2, it can be found that the precipitation rates of the essence samples 2 and 3 added with the plant antimicrobial peptide but not added with the chelating agent are both higher and have a small difference, which indicates that more hyaluronic acid precipitates can be separated out by adding the plant antimicrobial peptide. And the precipitation rate of the essence added with the chelating agent pentetate is lower than that of the essence added with the EDTA-disodium, which shows that the pentetate can better resolve the precipitate formed by the plant defensin and the hyaluronic acid than the EDTA-disodium.
The supernatant remaining after the filtration of the precipitate was used as a sample for this experiment, and the sample was examined by GPC-MALLS method and the measurement was repeated 3 times, and the results are shown in Table 3.
The experimental method comprises the following steps: a GPC unit infusion pump; eighteen-angle laser light scattering instrument (wyattdawn heleos ii, usa); a differential refractometer detector (OptilabT-rex). Chromatographic conditions of column, Japanese Shodex OHpakSB-806HQ tandem SB-804HQ (8.0 mm. times.300 mm, 13 μm); mobile phase, ultra pure water (0.02% sodium azide), 0.22 μm filter membrane filtration, pH 6; flow rate 1.0mL/min－1(ii) a The temperature of the column oven is 40 ℃; the sample volume is 100 mu L; MW measurement range: 200-.
TABLE 3 HA molecular weight distribution results for the different formula compositions of the serum
Combining with the experimental data of the precipitation rate, the experiment finds that in the essence liquid sample added with the plant antibacterial peptide, more HA precipitates separated out by adding the plant antibacterial peptide are high-molecular-weight HA precipitates. In the essence sample further added with pentetate, the sample with lower precipitation rate and the essence with higher content of low molecular weight HA, which indicates that most of low molecular weight HA precipitates can be analyzed by adding pentetate. Further, when the mass ratio of the added hyaluronic acid, the plant defensin and the pentetate is 5: 3: 1, the content of low molecular weight HA in the essence sample in the ratio is higher than that in other ratios or the essence without the pentetate, which means that the pentetate is added and the hyaluronic acid, the plant defensin and the pentetate reach a certain ratio, so that the precipitate can be resolved into the essence with higher content of low molecular weight HA.
Example 3 antimicrobial and preservative Property test
Preparing a mixed bacterial solution for testing: the strains were inoculated in a suitable medium, bacteria were cultured at 37 ℃ for 48h, and fungi were cultured at 28 ℃ for 72 h. Selecting appropriate amount of bacterial colony in sterilized normal saline, and making into mixed bacteria with certain concentration (bacterial colony number is in108CFU/mL) or mixed fungus suspension (colony count is 10)7CFU/mL) and storing at 4 ℃ for later use.
Methods for testing the effectiveness of preservatives using a one-time microbial challenge test. 100mL of each test sample essence in example 1 was weighed, 1mL of mixed bacterial or mixed fungal suspension was added, and then mixed well. Ensuring that the bacteria content of the sample added with the bacteria suspension is 10 per milliliter6Adding the mixture into a sample of the fungus suspension at a ratio of 10 bacteria/gram sample, wherein the ratio of CFU/mL is about 105CFU/mL or so. Samples were taken at 0, 7, 14, 21 and 28 days post inoculation for analysis: accurately weighing 2mL of sample, adding the sample into a sterilized conical flask containing glass beads, adding 18mL of sterilized normal saline, fully shaking and uniformly mixing, wherein the suspension is a 1: 10 diluent; the bacteria content of the test article was counted by plate pour-on method. The test was conducted to evaluate the effect of the preservative according to the CTFA method, and the evaluation criteria of the test were: if the total number of colonies of the sample after adding the bacteria is less than or equal to 100CFU/mL on the 7 th day, the total number is gradually reduced until no increase occurs in 28 days, and the preservative effect is excellent; if the total number of colonies of the sample after adding bacteria is less than or equal to 1000CFU/mL on the 7 th day, the total number is gradually reduced until no increase occurs in 28 days, the test is just passed, and the antiseptic effect is qualified; if the total number of colonies is more than 1000CFU/mL at 7 days after the addition of the bacteria, the preservative is considered to be ineffective and has poor preservative effect.
TABLE 428 day microbial (bacterial) challenge test results (CFU/mL)
TABLE 528 day microbial (fungal) challenge test results (CFU/mL)
According to experimental data, the essence added with the preservative plant defensin and the chelating agent pentetate pentasodium has better antibacterial and antiseptic properties, and is higher than other essences without the plant defensin or pentetate pentasodium.
Example 4 measurement of transdermal absorption of GSH in Ex vivo skin
4.1 Standard Curve construction (HPLC method)
Chromatographic conditions are as follows: a chromatographic column: AgilentZorbaxSB-Aq, the mobile phase is a binary gradient mobile phase system A: 0.025% monopotassium phosphate (pH 3.8); b: methanol, flow rate 1.0mL/min, sample volume 20 uL, column temperature 30 ℃, detection wavelength: 210 nm.
Preparation of a standard solution: accurately weighing GSH 10mg, placing in 10mL measuring flask, dissolving and diluting blank skin receiving solution to scale, shaking, and making into stock solution. Precisely measuring 0.1 mL, 0.5 mL, 2.5 mL, 5.0 mL and 10.0mL of stock solutions, placing in a 10mL measuring flask, and diluting to constant volume with blank skin receiving solution to obtain reference solutions of 1.0, 5.0, 25.0, 50.0 and 100.0 ug/mL.
Establishing a standard curve: precisely measuring 1mL of the reference solution, adding 1mL of 1mg/mLDTNB solution, vortexing for 3min, injecting 20 μ L of the reaction solution into a high performance liquid chromatograph, and recording the chromatogram. Linear regression was performed with GSH mass concentration (ug/mL) as abscissa C and peak area a as ordinate.
The results are shown in fig. 1, which shows that GSH has a good linear relationship in the skin-receiving solution, and the linear regression equation is a 16512C +36189 (r)2＝0.9998)。
4.2 transdermal absorption of GSH in vitro
The analytical method is the same as 4.1. The Content (CX) in the permeation solution was calculated from the peak area of GSH and was in ug/mL.
The skin of the treated mouse with the abdominal hair removed was cut and fixed on a diffusion cell, and 1mL of the essence of all the samples of the examples was added to the supply cell. The receiving solution is a 20% ethanol physiological saline solution, and the dermal side is in complete contact with the receiving solution, and the stratum corneum faces the supply tank. The volume of the receiving solution is 9mL, and the effective diffusion area is 6.55cm2The magnetic stirring speed is 500r/min, and the water bath temperature is (37 +/-0.5) DEG C. Respectively 1, 2, 4, 6,8. At 10, 12, and 24 hours, 1mL of the receiving solution was taken out of the receiving cell, and an equal amount of the receiving solution was added to the receiving cell. Taking out 1mL of receiving solution, adding 1mL of DTNB solution, reacting for 3min by vortex, and filtering with 0.45 μm microporous membrane before sample injection. Each sample was tested in parallel 3 times, and the cumulative permeation per unit area Q was calculated according to the following formula1/ug·cm-2，Q1(content (CX) × 6.55)/9.
As shown in FIG. 2, the transdermal absorption amount of GSH in the serum sample with high content of low molecular weight HA is higher than that in the serum sample with high content of high molecular weight HA, wherein the cumulative penetration amount of GSH in the No. 1-9 serum after 24h is 200.55 μ g/cm2、77.04μg/cm2、84.1μg/cm2、190.4μg/cm2、311.8μg/cm2、326.1μg/cm2、303.6μg/cm2、212.6μg/cm2、89.3μg/cm2。
By combining the fact that the content of the low-molecular-weight HA in the essence 6 in the example 2 is high, and the transdermal absorption amount of the GSH of the essence 6 in the experiment is also high, it is shown that the plant defensin and pentetate can be used together in a certain proportion to remove most of the high-molecular-weight HA and leave the low-molecular-weight HA with high content, so that the transdermal absorption performance of the GSH is greatly improved. On the basis, the essence 6 prepared by the invention has better antibacterial and antiseptic properties. When the mass ratio of the hyaluronic acid to the plant defensin to the chelating agent pentetate is 5: 3: 1, the reduced glutathione has high bioavailability, and the product which can promote transdermal absorption of GSH to improve bioavailability, has whitening and moisturizing functions and has excellent antibacterial and antiseptic properties is obtained.
Compared with other common chemical preservatives, such as phenethyl alcohol, hydroxy benzyl ester and the like, the added plant antibacterial peptide has the advantages of biological environmental protection, no residual hidden danger, almost no irritation and toxicity to skin and better antibacterial effect. Compared with other common plant antibacterial peptides such as rubber protein, Knottins and the like, the plant antibacterial peptide with strong cations can better generate electrostatic interaction with hyaluronic acid to generate precipitates.
In conclusion, the facial mask essence containing hyaluronic acid prepared by the invention has excellent whitening, moisturizing and antioxidant functions, excellent antibacterial and antiseptic properties and high bioavailability of reduced glutathione, and is a green and safe facial mask essence.
Claims (8)
1. The facial mask essence containing hyaluronic acid comprises water, reduced glutathione, hyaluronic acid and other auxiliary materials, and is characterized by further comprising plant antibacterial peptide with cations.
2. The mask essence containing hyaluronic acid according to claim 1, further comprising a chelating agent.
3. The mask essence containing hyaluronic acid according to claim 2, wherein the cationic plant antimicrobial peptide is a plant defensin.
4. The mask essence containing hyaluronic acid according to claim 3, wherein the chelating agent is pentasodium pentetate.
5. The mask essence containing hyaluronic acid as claimed in claim 4, wherein the mass ratio of hyaluronic acid to plant defensin to pentetate is 5: 3: 1.
6. the mask essence containing hyaluronic acid according to claim 1, wherein the essence comprises the following components: 0.1 to 0.8 percent of reduced glutathione, 0.2 to 1 percent of hyaluronic acid, 0.05 to 0.15 percent of chelating agent, 0.1 to 1 percent of plant antibacterial peptide with cations, 21 to 26 percent of other auxiliary materials and the balance of water.
7. The mask essence containing hyaluronic acid according to claim 1, wherein the other adjuvants comprise: surfactant, thickener, humectant, acidity regulator and essence.
8. The mask essence containing hyaluronic acid according to claim 1, wherein the essence comprises the following components: 0.25% of reduced glutathione, 0.5% of hyaluronic acid, 0.1% of pentetate, 0.3% of plant defensin, 25.35% of other auxiliary materials and the balance of water.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105622741A (en) * | 2014-10-28 | 2016-06-01 | 无锡灵锡医疗器械科技有限公司 | Preparation method of composition for contact lens surface antibacterial coating and application method |
| CN109692130A (en) * | 2019-01-30 | 2019-04-30 | 威海同丰海洋生物科技有限公司 | A kind of facial mask liquid and preparation method thereof containing alexin |
| CN111686032A (en) * | 2020-05-29 | 2020-09-22 | 广州新诚生物科技有限公司 | Essence, preparation method and facial mask |
| CN112316203A (en) * | 2020-11-06 | 2021-02-05 | 黄石瀚海新材料科技有限公司 | Cationic antibacterial peptide and hyaluronic acid composite hydrogel and preparation method thereof |
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- 2021-10-11 CN CN202111182105.XA patent/CN113876624A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105622741A (en) * | 2014-10-28 | 2016-06-01 | 无锡灵锡医疗器械科技有限公司 | Preparation method of composition for contact lens surface antibacterial coating and application method |
| CN109692130A (en) * | 2019-01-30 | 2019-04-30 | 威海同丰海洋生物科技有限公司 | A kind of facial mask liquid and preparation method thereof containing alexin |
| CN111686032A (en) * | 2020-05-29 | 2020-09-22 | 广州新诚生物科技有限公司 | Essence, preparation method and facial mask |
| CN112316203A (en) * | 2020-11-06 | 2021-02-05 | 黄石瀚海新材料科技有限公司 | Cationic antibacterial peptide and hyaluronic acid composite hydrogel and preparation method thereof |
Non-Patent Citations (1)
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