CN113368530A - Extraction method and application of polygonatum cyrtonema extract - Google Patents
Extraction method and application of polygonatum cyrtonema extract Download PDFInfo
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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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
- A61K8/96—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution
- A61K8/97—Cosmetics or similar toiletry preparations characterised by the composition containing materials, or derivatives thereof of undetermined constitution from algae, fungi, lichens or plants; from derivatives thereof
- A61K8/9783—Angiosperms [Magnoliophyta]
- A61K8/9794—Liliopsida [monocotyledons]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61P—SPECIFIC THERAPEUTIC ACTIVITY OF CHEMICAL COMPOUNDS OR MEDICINAL PREPARATIONS
- A61P29/00—Non-central analgesic, antipyretic or antiinflammatory agents, e.g. antirheumatic agents; Non-steroidal antiinflammatory drugs [NSAID]
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61Q—SPECIFIC USE OF COSMETICS OR SIMILAR TOILETRY PREPARATIONS
- A61Q19/00—Preparations for care of the skin
- A61Q19/08—Anti-ageing preparations
Abstract
The invention discloses an extraction method and application of polygonatum cyrtonema extracting solution. The extraction method of polygonatum cyrtonema extract comprises the following steps: leaching rhizome powder of polygonatum cyrtonema in water to obtain a leaching solution; and carrying out reduced pressure concentration on the leaching liquor to obtain the polygonatum cyrtonema extracting solution. The polygonatum cyrtonema extract obtained by extracting water as an extraction solvent mainly comprises polysaccharide and contains a small amount of protein and polyphenol; the polygonatum cyrtonema extracting solution extracted by the extraction method provided by the invention is applied to cosmetics and has multiple effects of moisture preservation, inflammation resistance, oxidation resistance and the like. The extraction method of polygonatum cyrtonema extracting solution is simple to operate and mild in condition, and the obtained polygonatum cyrtonema extracting solution has good stability and applicability when being applied to cosmetics, and has good industrial application prospect.
Description
Technical Field
The invention relates to an extraction method and application of polygonatum cyrtonema extract, belonging to the technical field of cosmetics.
Background
Rhizoma polygonati is a perennial herb plant of the genus polygonatum of the family liliaceae, uses roots and stems as medicines, and is one of the plants which are homologous in medicine and food in China. The sealwort is mainly divided into three types, namely polygonatum kingianum, sealwort and polygonatum cyrtonema. Polygonatum cyrtonema is widely distributed in China, and mainly focuses on Anhui, Hunan innovation, Guizhou Zunyi, Yunnan and other places. Polygonatum cyrtonema contains various active substances such as polysaccharide, brass, polyphenol, lignin, alkaloid and the like, and has pharmacological effects of resisting inflammation, inhibiting bacteria, resisting oxidation, enhancing immunity and the like.
With the development of economy, consumers prefer safe and green natural cosmetics, plant extracts as cosmetic raw materials gradually occupy a large market, at present, polygonatum cyrtonema extracting solution is more applied to food, but is less developed and applied in cosmetics, and how to prepare the more effective polygonatum cyrtonema extracting solution which can be used in cosmetics becomes an important research direction.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the development and utilization of rhizoma Polygonati in cosmetics.
In order to solve the technical problems, the invention provides a method for extracting polygonatum cyrtonema extract, which comprises the following steps:
leaching rhizome powder of polygonatum cyrtonema in water to obtain a leaching solution; and carrying out reduced pressure concentration on the leaching liquor to obtain polygonatum cyrtonema extracting solution.
Preferably, the using amount ratio of polygonatum cyrtonema rhizome powder to water is 1 g: 10-30 mL; the leaching temperature is 60-100 ℃, and the leaching time is 1-5 h.
The invention also provides polygonatum cyrtonema extracting solution obtained by the polygonatum cyrtonema extracting solution extracting method, wherein the concentration of the polygonatum cyrtonema extracting solution is 0.2-0.3 g/mL; the polygonatum cyrtonema extracting solution comprises polysaccharide, protein and polyphenol; the mass ratio of the polysaccharide to the protein to the polyphenol is 33.78-34.42: 0.038-0.050: 0.211 to 0.232.
The invention also provides application of the polygonatum cyrtonema extracting solution extracted by the polygonatum cyrtonema extracting solution extracting method in cosmetics.
The invention also provides a toning lotion containing polygonatum cyrtonema extract, which comprises 1-4% of polygonatum cyrtonema extract, 0.01-0.03% of hyaluronic acid, 7-9% of glycerol, 6-10% of propylene glycol, 0.1-0.4% of preservative GPL and the balance of water in percentage by mass; the polygonatum cyrtonema extracting solution is extracted by the polygonatum cyrtonema extracting method of claim 1 or 2.
The invention also provides an emulsion containing polygonatum cyrtonema extracting solution, which comprises, by mass, 21-1.5% of stearyl alcohol polyoxyethylene ether, 211-2% of stearyl alcohol polyoxyethylene ether, 0.1-1% of hexadecanol-octadecanol, 2.0-4.0% of simethicone, 3.0-5.0% of octyl/decyl triglyceride, 3.0-5.0% of white oil, 0.01-0.05% of 2, 6-di-tert-butyl-4-methylphenol, 1-4% of polygonatum cyrtonema extracting solution, 1-5% of propylene glycol, 3-8% of glycerol, 8-12% of carbomer, 0.1-0.4% of preservative GPL, and the balance of water; the pH value of the emulsion is 7-8; the polygonatum cyrtonema extracting solution is extracted by the polygonatum cyrtonema extracting method of claim 1 or 2.
Preferably, the preparation method comprises the following steps:
mixing and melting hard alcohol polyoxyethylene ether-2, hard alcohol polyoxyethylene ether-21, hexadecanol-octadecanol, simethicone, octyl/decyl triglyceride, white oil and 2, 6-di-tert-butyl-4-methylphenol to obtain an oil phase; mixing water, Polygonatum sibiricum extract, propylene glycol, glycerol and carbomer to obtain a water phase; and adding the oil phase into the water phase, homogenizing, adding a preservative, and adjusting the pH value to 7-8 to obtain the polygonatum cyrtonema extract-containing emulsion.
The invention also provides cream containing polygonatum cyrtonema extracting solution, which comprises, by mass, 21-2% of stearyl alcohol polyoxyethylene ether, 212-3% of stearyl alcohol polyoxyethylene ether, 0.5-1.5% of hexadecanol-octadecanol, 1-2% of glyceryl monostearate, 2.0-4.0% of simethicone, 2-4% of octyl/decyl triglyceride, 4-6% of white oil, 0.01-0.1% of 2, 6-di-tert-butyl-4-methylphenol, 1-4% of polygonatum cyrtonema extracting solution, 1-3% of propylene glycol, 3-8% of glycerol, 10-25% of carbomer, 0.1-0.3% of preservative GPL, and the balance of water; the pH value of the cream is 7-8; the polygonatum cyrtonema extracting solution is extracted by the polygonatum cyrtonema extracting method of claim 1 or 2.
Preferably, the preparation method comprises the following steps:
mixing and melting stearyl alcohol polyoxyethylene ether-2, stearyl alcohol polyoxyethylene ether-21, hexadecanol-octadecanol, simethicone, glyceryl monostearate, octyl/decyl triglyceride, white oil and 2, 6-di-tert-butyl-4-methylphenol to obtain an oil phase; mixing water, Polygonatum sibiricum extract, propylene glycol, glycerol and carbomer to obtain a water phase; and adding the oil phase into the water phase, homogenizing, adding a preservative, and adjusting the pH value to 7-8 to obtain the cream containing the polygonatum cyrtonema extracting solution.
More preferably, in the preparation method of the emulsion or cream containing polygonatum cyrtonema extract, the homogenization treatment temperature is 80-85 ℃, the rotation speed is 10000-110000 rpm, and the time is 1-3 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the invention adopts water as the extraction solvent, and overcomes the problem that the composition of the extraction liquid is changed when the aqueous solution of ethanol is adopted as the extraction solvent in the prior art;
2. the method can improve the content of polysaccharide in polygonatum cyrtonema extracting solution by taking water as an extraction solvent, and the polysaccharide has a wide molecular weight range, and the polygonatum cyrtonema extracting solution extracted by the extraction method has the mass ratio of polysaccharide, protein and polyphenol of (33.78-34.42): (0.038-0.050): (0.211-0.232);
3. the polygonatum cyrtonema extracting solution extracted by the invention is applied to cosmetics and has multiple effects of moisture preservation, inflammation resistance, oxidation resistance and the like; meanwhile, the extraction method provided by the invention is simple to operate and mild in condition, and the obtained polygonatum cyrtonema extracting solution has good stability and applicability when being applied to cosmetics, and has a good industrial application prospect.
Drawings
FIG. 1 shows VC clearance of hydroxyl radicals;
FIG. 2 shows the scavenging rate of Polygonatum cyrtonema extractive solution on hydroxyl radical;
FIG. 3 is a graph of VC for superoxide anion removal;
FIG. 4 shows the removal rate of superoxide anion by Polygonatum cyrtonema extractive solution;
FIG. 5 shows the scavenging rate of VC on hydrogen peroxide;
FIG. 6 shows the clearance of the Polygonatum cyrtonema extractive solution to hydrogen peroxide;
fig. 7 is the respiratory burst suppression rate of resveratrol;
FIG. 8 shows the respiratory burst suppression rate of Polygonatum cyrtonema extractive solution;
FIG. 9 shows the hygroscopic change rates of Polygonatum cyrtonema extractive solution and sorbitol;
FIG. 10 shows the change rate of moisturizing effect of Polygonatum cyrtonema extractive solution and sorbitol.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Example 1
A method for extracting polygonatum cyrtonema extract comprises the following steps:
step 1: washing and drying rhizomes of polygonatum cyrtonema with a deionized book, slicing, crushing and sieving to obtain 200-mesh rhizomes powder of polygonatum cyrtonema;
step 2: leaching 1.00g rhizome powder of polygonatum cyrtonema for 2h in 20.00mL hot water with the temperature of 80 ℃ to obtain leaching liquor; measuring molecular weight of the leaching solution by high performance anion chromatography, wherein the molecular weight distribution range is 3.696 × 103～1.017×106Da, concentrating the obtained leaching liquor in vacuum for 2-2.5 h at 55 ℃ and under the pressure of 220mbar to obtain Polygonatum cyrtonema extractive solution, and finallyThe final concentration is 0.25g/mL (meaning that 0.25g sample is extracted by deionized water and then is concentrated to 1mL in vacuum), the main components are polysaccharide, protein and polyphenol, the mass ratio is 34.26:0.043:0.223, and active substances such as flavone, amino acid, lignin, alkaloid and the like are also contained.
Example 2
A lotion containing Polygonatum cyrtonema extract:
the preparation raw materials comprise:
EXAMPLE 1 Polygonatum cyrtonema extractive solution 2 wt%
Hyaluronic acid 0.02 wt%
8 wt% of glycerol
Propylene glycol 7 wt%
Preservative GPL 0.2 wt%
The balance of water;
the preparation process comprises the following steps:
mixing water, Polygonatum cyrtonema extract, hyaluronic acid, glycerol and propylene glycol at 85 deg.C, stirring to obtain uniform solution system, and adding antiseptic GPL at room temperature to obtain cosmetic water containing Polygonatum cyrtonema extract.
Example 3
A lotion containing Polygonatum cyrtonema extract:
the preparation raw materials comprise:
EXAMPLE 1 Polygonatum cyrtonema extractive solution 3 wt%
Hyaluronic acid 0.02 wt%
8 wt% of glycerol
Propylene glycol 7 wt%
Preservative GPL 0.2 wt%
The balance of water;
the preparation process comprises the following steps:
mixing water, Polygonatum cyrtonema extract, hyaluronic acid, glycerol and propylene glycol at 85 deg.C, stirring to obtain uniform solution system, and adding antiseptic GPL at room temperature to obtain cosmetic water containing Polygonatum cyrtonema extract.
Example 4
An emulsion containing Polygonatum cyrtonema extract:
the preparation raw materials comprise:
stearyl alcohol polyoxyethylene Ether-21.2 wt%
Stearyl alcohol polyoxyethylene Ether-211.5 wt.%
Heptadeca-octadecanol 0.5 wt%
3.0 wt% of simethicone
Octyl/decyl triglyceride 4.0% by weight
White oil 3.0 wt%
0.05% by weight of 2, 6-di-tert-butyl-4-methylphenol (BHT)
EXAMPLE 1 Polygonatum cyrtonema extractive solution 2.0 wt%
2.0% by weight of propylene glycol
5.0 wt% of glycerin
Carbomer 10.0 wt%
Preservative GPL 0.2 wt%
The balance of water;
the pH value of the emulsion is 7.5;
the preparation process comprises the following steps:
mixing hard alcohol polyoxyethylene ether-2, hard alcohol polyoxyethylene ether-21, hexadecanol-octadecanol, simethicone, octyl/decyl triglyceride, white oil and 2, 6-di-tert-butyl-4-methylphenol, and melting at 85 ℃ to obtain an oil phase; mixing water, Polygonatum sibiricum extract, propylene glycol, glycerol and carbomer at 85 deg.C, and stirring to obtain water phase; and adding the oil phase into the water phase for homogenization treatment, wherein the homogenization treatment temperature is 85 ℃, the rotation speed is 10000rpm, and the time is 3min, adding a preservative after the homogenization treatment, and adjusting the pH value to 7.5 to obtain the emulsion containing the polygonatum cyrtonema extracting solution.
Example 5
An emulsion containing Polygonatum cyrtonema extract:
the preparation raw materials comprise:
stearyl alcohol polyoxyethylene Ether-21.2 wt%
Stearyl alcohol polyoxyethylene Ether-211.5 wt.%
Octadecanol 0.5 wt%
3.0 wt% of simethicone
Octyl/decyl triglyceride 4.0% by weight
White oil 3.0 wt%
0.05% by weight of 2, 6-di-tert-butyl-4-methylphenol (BHT)
EXAMPLE 1 Polygonatum cyrtonema extractive solution 3.0 wt%
2.0% by weight of propylene glycol
5.0 wt% of glycerin
Carbomer 10.0 wt%
Preservative GPL 0.2 wt%
The balance of water;
the pH value of the emulsion is 7.5;
the preparation process comprises the following steps:
mixing hard alcohol polyoxyethylene ether-2, hard alcohol polyoxyethylene ether-21, hexadecanol-octadecanol, simethicone, octyl/decyl triglyceride, white oil and 2, 6-di-tert-butyl-4-methylphenol, and melting at 85 ℃ to obtain an oil phase; mixing water, Polygonatum sibiricum extract, propylene glycol, glycerol and carbomer at 85 deg.C, and stirring to obtain water phase; and adding the oil phase into the water phase for homogenization treatment, wherein the homogenization treatment temperature is 85 ℃, the rotation speed is 10000rpm, and the time is 3min, adding a preservative after the homogenization treatment, and adjusting the pH value to 7.5 to obtain the emulsion containing the polygonatum cyrtonema extracting solution.
Example 6
A cream containing Polygonatum cyrtonema extractive solution:
the preparation raw materials comprise:
stearyl alcohol polyoxyethylene Ether-21.8 wt%
Stearyl alcohol polyoxyethylene Ether-212.2 wt.%
Hexadecanol-octadecanol 1.0 wt%
Glyceryl monostearate 1.0 wt%
2.0 wt% of simethicone
Octyl/decyl triglyceride 3.0 wt.%
White oil 5.0 wt%
0.05 wt% of 2, 6-di-tert-butyl-4-methylphenol
EXAMPLE 1 Polygonatum cyrtonema extractive solution 2.0 wt%
2.0% by weight of propylene glycol
5.0 wt% of glycerin
Carbomer 20.0 wt%
Preservative GPL 0.2 wt%
The balance of water;
the pH value of the cream is 7.5;
the polygonatum cyrtonema extracting solution is a polygonatum cyrtonema extracting solution;
the preparation process comprises the following steps:
mixing hard alcohol polyoxyethylene ether-2, hard alcohol polyoxyethylene ether-21, hexadecanol-octadecanol, dimethyl silicone oil, glyceryl monostearate, octyl/decyl triglyceride, white oil and 2, 6-di-tert-butyl-4-methylphenol, and melting at 85 ℃ to obtain an oil phase; mixing water, Polygonatum sibiricum extract, propylene glycol, glycerol and carbomer at 85 deg.C, and stirring to obtain water phase; and adding the oil phase into the water phase for homogenization treatment, wherein the homogenization treatment temperature is 85 ℃, the rotation speed is 10000rpm, and the time is 3min, adding a preservative after the homogenization treatment, and adjusting the pH value to 7.5 to obtain the cream containing the polygonatum cyrtonema extracting solution.
Example 7
A cream containing Polygonatum cyrtonema extractive solution:
the preparation raw materials comprise:
stearyl alcohol polyoxyethylene Ether-21.8 wt%
Stearyl alcohol polyoxyethylene Ether-212.2 wt.%
Hexadecanol-octadecanol 1.0 wt%
Glyceryl monostearate 1.0 wt%
2.0 wt% of simethicone
Octyl/decyl triglyceride 3.0 wt.%
White oil 5.0 wt%
0.05 wt% of 2, 6-di-tert-butyl-4-methylphenol
EXAMPLE 1 Polygonatum cyrtonema extractive solution 3.0 wt%
2.0% by weight of propylene glycol
5.0 wt% of glycerin
Carbomer 20.0 wt%
Preservative GPL 0.2 wt%
The balance of water;
the pH value of the cream is 7.5;
the preparation process comprises the following steps:
mixing hard alcohol polyoxyethylene ether-2, hard alcohol polyoxyethylene ether-21, hexadecanol-octadecanol, dimethyl silicone oil, glyceryl monostearate, octyl/decyl triglyceride, white oil and 2, 6-di-tert-butyl-4-methylphenol, and melting at 85 ℃ to obtain an oil phase; mixing water, Polygonatum sibiricum extract, propylene glycol, glycerol and carbomer at 85 deg.C, and stirring to obtain water phase; and adding the oil phase into the water phase for homogenization treatment, wherein the homogenization treatment temperature is 85 ℃, the rotation speed is 10000rpm, and the time is 3min, adding a preservative after the homogenization treatment, and adjusting the pH value to 7.5 to obtain the cream containing the polygonatum cyrtonema extracting solution.
Comparative example 1
Washing and drying rhizomes of polygonatum cyrtonema with a deionized book, slicing, crushing and sieving to obtain 200-mesh rhizomes powder of polygonatum cyrtonema;
adding 1.00g of radix et rhizoma Rhei Palmati powder into 20.00mL of 85% ethanol water solution, ultrasonic treating for 30min, volatilizing ethanol from the obtained leaching solution, and detecting molecular weight of 1.758 × 10 by high performance liquid chromatography3Da。
Test:
first, antioxidant capacity test
The polygonatum cyrtonema extract obtained in example 1 was tested for its antioxidant capacity by chemiluminescence, and the hydroxyl radical clearance, superoxide anion clearance, and hydrogen peroxide clearance were used as evaluation indices.
1. Hydroxyl radical scavenging rate
Adding 0.05mol/mL of Na2CO3The solution was mixed with 0.05mol/mL NaHCO3The solution was mixed to pH 8.5 as carbonate buffer with 1mmol/L luminol as 17: 1 is prepared into luminol-carbonate luminous working solution, and H with the concentration of 6 percent is prepared2O2The solution comprises 1mmol/L cuprous chloride solution and 1mmol/L phenanthroline solution. Sequentially injecting 10uL of Polygonatum cyrtonema extractive solutions with different concentrations (the concentrations are 0.78mg/mL and 0.78mg/mL respectively),1.56mg/mL, 3.13mg/mL, 6.25mg/mL, 12.5mg/mL, 25mg/mL), 10uL of 1mmol/L phenanthroline, 10uL of 6% H2O2150uL luminol-carbonate luminous working solution, 10uL 1mmol/L cuprous chloride, 3 compound holes arranged in each hole, a chemiluminescence instrument continuously recording experimental data for 15s, and recording the experimental data every 2s to obtain a peak value A1The blank control group uses deionized water to replace Polygonatum cyrtonema extractive solution to obtain peak value A0The clearance rate of VC on hydroxyl radical is taken as a positive control. The hydroxyl radical clearance equation is as follows:
clearance (%) - (1-A)1/A0)×100；
The results of VC on the clearance of hydroxyl radicals are shown in figure 1, and the results of Polygonatum cyrtonema extract on the clearance of hydroxyl radicals are shown in figure 2. From the results shown in FIGS. 1 to 2, it is understood that the IC50 value of VC obtained by SPSS regression analysis is 0.202mg/mL, and the scavenging ability of the Polygonatum sibiricum extract solution is equivalent to the scavenging ability of VC at a concentration of 0.202mg/mL when the dilution factor is 26.22.
2. Superoxide anion removal rate
Adding 0.05mol/mL of Na2CO3The solution was mixed with 0.05mol/mL NaHCO3The solution was mixed to pH 10 as carbonate buffer with 1mmol/L luminol as 2: 1 to prepare luminol-carbonate luminous working solution, and 0.0625mmol/L pyrogallol. During measurement, 10uL of polygonatum cyrtonema extract (the concentrations are respectively 0.78mg/mL, 1.56mg/mL, 3.13mg/mL, 6.25mg/mL, 12.5mg/mL and 25mg/mL), 10uL of 0.0625mmol/L pyrogallol and 150uL of luminol-carbonate luminescence working solution are sequentially injected into a luminescence pool. Each hole is provided with 3 multiple holes, a chemiluminescence apparatus is arranged to continuously record experimental data for 30s, and the experimental data is recorded every 2s to obtain a peak value A1The blank control group uses deionized water to replace Polygonatum cyrtonema extractive solution to obtain peak value A0The clearance rate of VC to superoxide anion is taken as a positive control. The superoxide anion clearance equation is as follows:
clearance (%) - (1-A)1/A0)×100；
The results of VC on the removal rate of superoxide anions are shown in FIG. 3, and the results of Polygonatum cyrtonema extract on the removal rate of superoxide anions are shown in FIG. 4. From the results shown in FIGS. 3 to 4, it is understood that the IC50 value of VC obtained by SPSS regression analysis is 0.257mg/mL, and the scavenging ability of the Polygonatum sibiricum extract solution is equivalent to the scavenging ability of VC at a concentration of 0.257mg/mL when the dilution factor is 59.32.
3、H2O2Clearance rate
Adding 0.05mol/mL of Na2CO3The solution was mixed with 0.05mol/mL NaHCO3The solution was mixed to pH 9.5 as carbonate buffer with 1mmol/L luminol as 17: 1 is prepared into luminol-carbonate luminous working solution, and H with the concentration of 6 percent is prepared2O2And (3) solution. During measurement, 10uL of Polygonatum cyrtonema extractive solutions (with concentrations of 0.5mg/mL, 1mg/mL, 1.5mg/mL, 2.0mg/mL, 2.5mg/mL and 3mg/mL respectively) and 10uL of 6% H were sequentially injected into a luminescence pool2O2Solution and 150uL luminol-carbonate luminous working solution. Each hole is provided with 3 multiple holes, a chemiluminescence apparatus is arranged to continuously record experiment data for 5s, and the experiment data is recorded every 1.5s to obtain a peak value A1The blank control group uses deionized water to replace Polygonatum cyrtonema extractive solution to obtain peak value A0The clearance of VC to hydrogen peroxide is taken as a positive control. The superoxide anion clearance equation is as follows:
clearance (%) - (1-A)1/A0)×100；
The results of the removal rate of hydrogen peroxide by VC are shown in FIG. 5, and the results of the removal rate of superoxide anion by Polygonatum cyrtonema extractive solution are shown in FIG. 6. From the results shown in FIGS. 5 to 6, it is understood that the IC50 value of VC obtained by SPSS regression analysis is 0.175mg/mL, and the scavenging ability of Polygonatum cyrtonema extract is equivalent to that of VC with a concentration of 0.175mg/mL when the dilution factor of Polygonatum cyrtonema extract is 566.16, so that Polygonatum cyrtonema extract has a strong scavenging ability to hydrogen peroxide.
Second, anti-inflammatory Activity test
The respiratory burst method is adopted to determine the anti-inflammatory effect of the polygonatum cyrtonema extract extracted in the example 1, and Raw264.7 macrophages generate a large amount of active oxygen and inflammatory factors under the stimulation of PMA to cause inflammatory reaction. In general, luminol and oxide have very rapid chemiluminescence reaction in the presence of certain catalysts, the intensity of respiratory burst is indicated by capturing a luminescence value, and the intensity of respiratory burst inhibition is the intensity of anti-inflammation.
Adding 180uL of Raw264.7 macrophage suspension with the cell density of 5 multiplied by 105/mL, 10uL of polygonatum multiflorum extracting solution (the concentrations are respectively 10mg/mL, 20mg/mL, 30mg/mL, 40mg/mL and 50mg/mL) with different concentrations and 60uL of luminol luminous working solution into a luminous pool, mixing uniformly, and quickly adding 2.5uL of PMA with the concentration of 0.02 mg/mL. Setting the temperature of the chemiluminescence apparatus at 37 deg.C, recording one round of experimental data per minute, continuously measuring for 30min, and measuring peak value A1Setting 3 multiple wells for each sample, averaging, using PBS to replace Polygonatum cyrtonema extractive solution for control group, and determining peak value A0Taking the respiratory burst inhibition rate of resveratrol as a positive control, the inhibition rate formula is as follows:
inhibition ratio (%) - (1-A)1/A0)×100；
The respiratory burst inhibition rate of resveratrol is shown in fig. 7, and the respiratory burst inhibition rate of polygonatum cyrtonema extract is shown in fig. 8. From the results in fig. 7 to 8, it is understood that the IC50 value of resveratrol obtained by SPSS regression analysis is 1.083mg/mL, and the removal ability of resveratrol with a concentration of 1.083mg/mL is comparable to that of polygonatum cyrtonema extract solution diluted by a factor of 6.05.
Third, testing moisture absorption and retention ability
Freeze-drying the polygonatum cyrtonema extracting solution obtained in the example 1 to obtain polygonatum cyrtonema crude polysaccharide; taking 0.2g crude polysaccharide of Polygonatum cyrtonema Hua, and recording as M0Placing in a constant temperature and humidity cabinet, controlling relative humidity at 81% and temperature at 25 deg.C, measuring weight at regular intervals until reaching moisture absorption saturation state (constant weight), and recording the weight as MnTransferring to a constant temperature and humidity box with a relative humidity of 43% and a temperature of 25 ℃, and recording the weight before transferring as H0Measuring the weight of the sample at intervals, stopping weighing after constant weight, and recording as HnCommercial sorbitol was used as a positive control. The moisture absorption rate and the moisture retention rate formula are as follows:
moisture absorption (%) (M)n-M0)/M0×100；
The results of the polygonatum cyrtonema extract and the change rate of sorbitol in moisture absorption are shown in fig. 9, and it can be seen from fig. 9 that the polygonatum cyrtonema extract has a moisture absorption capacity significantly better than that of commercially available sorbitol, and almost reaches a saturated state when the moisture absorption time is 48 hours, the polygonatum cyrtonema extract has a moisture absorption rate of 30.25%, the commercially available sorbitol has a moisture absorption rate of 6.06%, and the polygonatum cyrtonema extract has a moisture absorption rate 24.19% higher than that of commercially available sorbitol.
Moisture retention rate (%) ═ Hn/H0×100；
The results of the moisturizing change rates of the polygonatum cyrtonema extract and sorbitol are shown in fig. 10, and it is understood from fig. 10 that when the moisturizing time is 48 hours, the moisturizing rate of the polygonatum cyrtonema extract is 83.93%, the moisturizing rate of commercially available sorbitol is 77.4%, and the moisturizing rate of the polygonatum cyrtonema extract is 6.53% higher than that of commercially available sorbitol. Combining the results of fig. 9 and fig. 10, the moisture absorption rate and moisture retention rate of the polygonatum cyrtonema extract are both significantly superior to those of commercially available sorbitol.
Fourth, safety test
Randomly selecting 30 volunteers with age of 18-60 years and no serious skin damage, dripping 0.1g of the lotion, emulsion and cream obtained in examples 2-7 on a filter paper sheet, and placing the filter paper sheet in a spot tester hole to obtain a test sample. Each test sample is provided with a blank control sample, namely 0.1g of distilled water is dripped on a filter paper sheet, and then the filter paper sheet is placed in a hole of a spot tester for control to obtain the control sample. The flexed sides of the two forearms of the human body are selected as test areas, and the spot tester is fixedly pasted on the flexed sides of the two forearms of the volunteer by using a non-irritant adhesive tape. The test period was 24h, during which the volunteer could not remove the plaque tester or expose the test area to water. After 24h, the skin states of observers are negative, and the samples are non-irritant, so that the toning lotion, the emulsion and the cream containing the polygonatum cyrtonema extract in the examples 2-7 are safe.
Fifth, stability test
1. Cold stability
And (3) placing the sample obtained in the embodiment 2-7 in a refrigerator at-15 ℃ for 24h, taking out the sample, placing the sample at room temperature, comparing the sample with the sample at room temperature, and observing whether the sample is layered or not.
2. Thermal stability
And (3) placing the sample obtained in the embodiment 2-7 in a constant temperature incubator at 40 ℃ for 24h, taking out the sample, placing the sample to return to room temperature, comparing the sample with the sample at room temperature, and observing whether the sample is layered or not.
3. Cold and hot alternation stability
And (3) placing the sample obtained in the example 2-7 in a refrigerator at-15 ℃ for 24h, taking out, immediately placing in a constant-temperature incubator at 40 ℃ for 24h, taking out, comparing with the sample at room temperature, and observing whether the sample is layered or not.
4. Centrifugal experiment
And (3) placing the sample obtained in the embodiment 2-7 in a centrifuge, and observing the separation and layering conditions of the product after performing an experiment at the rotating speed of 2000rpm for 30 min.
By investigating cold stability, heat stability, cold-hot alternating stability and centrifugal stability of the prepared lotion, emulsion and cream containing the polygonatum cyrtonema extracting solution, the phenomenon of layering does not occur in the lotion, emulsion and cream containing the polygonatum cyrtonema extracting solution, and the result shows that the lotion, emulsion and cream containing the polygonatum cyrtonema extracting solution have good stability.
The above-described embodiments are only preferred embodiments of the present invention, and are not intended to limit the present invention in any way and substantially, it should be noted that those skilled in the art may make several modifications and additions without departing from the scope of the present invention, which should also be construed as a protection scope of the present invention.
Claims (10)
1. A method for extracting polygonatum cyrtonema extract is characterized by comprising the following steps:
leaching rhizome powder of polygonatum cyrtonema in water to obtain a leaching solution; and carrying out reduced pressure concentration on the leaching liquor to obtain polygonatum cyrtonema extracting solution.
2. The method for extracting polygonatum cyrtonema extracting solution according to claim 1, wherein the ratio of polygonatum cyrtonema rhizome powder to water is 1 g: 10-30 mL; the leaching temperature is 60-100 ℃, and the leaching time is 1-5 h.
3. The polygonatum cyrtonema extracting solution extracted by the polygonatum cyrtonema extracting solution extracting method of claim 1 or 2, wherein the concentration of the polygonatum cyrtonema extracting solution is 0.2-0.3 g/mL; the polygonatum cyrtonema extracting solution comprises polysaccharide, protein and polyphenol; the mass ratio of the polysaccharide to the protein to the polyphenol is 33.78-34.42: 0.038-0.050: 0.211 to 0.232.
4. The use of the polygonatum cyrtonema extracting solution extracted by the polygonatum cyrtonema extracting solution extracting method of claim 1 or 2 in cosmetics.
5. The toning lotion containing polygonatum cyrtonema extract is characterized by comprising 1-4% of polygonatum cyrtonema extract, 0.01-0.03% of hyaluronic acid, 7-9% of glycerol, 6-10% of propylene glycol, 0.1-0.4% of preservative GPL and the balance of water in percentage by mass; the polygonatum cyrtonema extracting solution is extracted by the polygonatum cyrtonema extracting method of claim 1 or 2.
6. An emulsion containing polygonatum cyrtonema extract is characterized by comprising, by mass, 21-1.5% of stearyl alcohol polyoxyethylene ether, 211-2% of stearyl alcohol polyoxyethylene ether, 0.1-1% of hexadecanol-octadecanol, 2.0-4.0% of simethicone, 3.0-5.0% of octyl/decyl triglyceride, 3.0-5.0% of white oil, 0.01-0.05% of 2, 6-di-tert-butyl-4-methylphenol, 1-4% of polygonatum cyrtonema extract, 1-5% of propylene glycol, 3-8% of glycerol, 8-12% of carbomer, 0.1-0.4% of preservative GPL, and the balance of water; the pH value of the emulsion is 7-8; the polygonatum cyrtonema extracting solution is extracted by the polygonatum cyrtonema extracting method of claim 1 or 2.
7. The emulsion of claim 6, wherein the preparation method comprises the following steps:
mixing and melting hard alcohol polyoxyethylene ether-2, hard alcohol polyoxyethylene ether-21, hexadecanol-octadecanol, simethicone, octyl/decyl triglyceride, white oil and 2, 6-di-tert-butyl-4-methylphenol to obtain an oil phase; mixing water, Polygonatum sibiricum extract, propylene glycol, glycerol and carbomer to obtain a water phase; and adding the oil phase into the water phase, homogenizing, adding a preservative, and adjusting the pH value to 7-8 to obtain the polygonatum cyrtonema extract-containing emulsion.
8. A cream containing polygonatum cyrtonema extracting solution is characterized by comprising, by mass, 21-2% of stearyl alcohol polyoxyethylene ether, 212-3% of stearyl alcohol polyoxyethylene ether, 0.5-1.5% of hexadecanol-octadecanol, 1-2% of glyceryl monostearate, 2.0-4.0% of simethicone, 2-4% of octyl/decyl triglyceride, 4-6% of white oil, 0.01-0.1% of 2, 6-di-tert-butyl-4-methylphenol, 1-4% of polygonatum cyrtonema extracting solution, 1-3% of propylene glycol, 3-8% of glycerol, 10-25% of carbomer, 0.1-0.3% of preservative GPL and the balance of water; the pH value of the cream is 7-8; the polygonatum cyrtonema extracting solution is extracted by the polygonatum cyrtonema extracting method of claim 1 or 2.
9. The cream containing polygonatum cyrtonema extract of claim 8, wherein the preparation method comprises the following steps:
mixing and melting stearyl alcohol polyoxyethylene ether-2, stearyl alcohol polyoxyethylene ether-21, hexadecanol-octadecanol, simethicone, glyceryl monostearate, octyl/decyl triglyceride, white oil and 2, 6-di-tert-butyl-4-methylphenol to obtain an oil phase; mixing water, Polygonatum sibiricum extract, propylene glycol, glycerol and carbomer to obtain a water phase; and adding the oil phase into the water phase, homogenizing, adding a preservative, and adjusting the pH value to 7-8 to obtain the cream containing the polygonatum cyrtonema extracting solution.
10. The polygonatum cyrtonema extracting solution-containing emulsion according to claim 7 or the polygonatum cyrtonema extracting solution-containing cream according to claim 9, wherein the temperature of the homogenization treatment is 80-85 ℃, the rotation speed is 10000-110000 rpm, and the time is 1-3 min.
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