CN116178586A - Application of bletilla striata polysaccharide in preparation of product with moisturizing effect - Google Patents
Application of bletilla striata polysaccharide in preparation of product with moisturizing effect Download PDFInfo
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- CN116178586A CN116178586A CN202310329685.3A CN202310329685A CN116178586A CN 116178586 A CN116178586 A CN 116178586A CN 202310329685 A CN202310329685 A CN 202310329685A CN 116178586 A CN116178586 A CN 116178586A
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- 150000004676 glycans Chemical class 0.000 title claims abstract description 159
- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 159
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 159
- 241001313857 Bletilla striata Species 0.000 title claims abstract description 143
- 230000003020 moisturizing effect Effects 0.000 title claims abstract description 23
- 238000002360 preparation method Methods 0.000 title abstract description 4
- 238000000605 extraction Methods 0.000 claims abstract description 88
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 86
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000000047 product Substances 0.000 claims abstract description 23
- 239000006228 supernatant Substances 0.000 claims abstract description 22
- 239000000843 powder Substances 0.000 claims abstract description 21
- 238000001556 precipitation Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 4
- 239000000243 solution Substances 0.000 claims description 52
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 38
- 239000002244 precipitate Substances 0.000 claims description 32
- 150000001450 anions Chemical class 0.000 claims description 21
- 238000004440 column chromatography Methods 0.000 claims description 18
- 239000011780 sodium chloride Substances 0.000 claims description 18
- 239000007788 liquid Substances 0.000 claims description 12
- 239000003480 eluent Substances 0.000 claims description 10
- 238000000746 purification Methods 0.000 claims description 5
- 238000000926 separation method Methods 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 2
- 239000006071 cream Substances 0.000 claims description 2
- 238000001035 drying Methods 0.000 claims description 2
- 239000008269 hand cream Substances 0.000 claims description 2
- 239000006210 lotion Substances 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- 238000012423 maintenance Methods 0.000 claims 1
- 238000010521 absorption reaction Methods 0.000 abstract description 11
- 241000196324 Embryophyta Species 0.000 abstract description 2
- 239000012153 distilled water Substances 0.000 description 18
- 238000004108 freeze drying Methods 0.000 description 16
- 238000000034 method Methods 0.000 description 15
- 230000014759 maintenance of location Effects 0.000 description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 8
- 238000001914 filtration Methods 0.000 description 8
- 238000002156 mixing Methods 0.000 description 8
- 239000000203 mixture Substances 0.000 description 8
- 230000001376 precipitating effect Effects 0.000 description 8
- 238000010298 pulverizing process Methods 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
- 238000004090 dissolution Methods 0.000 description 5
- 239000004909 Moisturizer Substances 0.000 description 4
- 229920002472 Starch Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000001333 moisturizer Effects 0.000 description 4
- 235000019698 starch Nutrition 0.000 description 4
- 239000008107 starch Substances 0.000 description 4
- 229920001661 Chitosan Polymers 0.000 description 3
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 description 3
- 239000008103 glucose Substances 0.000 description 3
- 235000011187 glycerol Nutrition 0.000 description 3
- 239000003906 humectant Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 230000008961 swelling Effects 0.000 description 3
- 241001313855 Bletilla Species 0.000 description 2
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 2
- 238000002835 absorbance Methods 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
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- 239000000126 substance Substances 0.000 description 2
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical group O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 description 1
- WQZGKKKJIJFFOK-QTVWNMPRSA-N D-mannopyranose Chemical compound OC[C@H]1OC(O)[C@@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-QTVWNMPRSA-N 0.000 description 1
- 229920002581 Glucomannan Polymers 0.000 description 1
- 206010062717 Increased upper airway secretion Diseases 0.000 description 1
- 208000019693 Lung disease Diseases 0.000 description 1
- 241000233855 Orchidaceae Species 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 208000007107 Stomach Ulcer Diseases 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 238000005571 anion exchange chromatography Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000000740 bleeding effect Effects 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001684 chronic effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
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- 238000007865 diluting Methods 0.000 description 1
- 239000000839 emulsion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000001815 facial effect Effects 0.000 description 1
- 201000005917 gastric ulcer Diseases 0.000 description 1
- 229940046240 glucomannan Drugs 0.000 description 1
- 238000005469 granulation Methods 0.000 description 1
- 230000003179 granulation Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 208000026435 phlegm Diseases 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- -1 small molecule compounds Chemical class 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000012086 standard solution Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
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- 238000005292 vacuum distillation Methods 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/0003—General processes for their isolation or fractionation, e.g. purification or extraction from biomass
-
- 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
-
- 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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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Animal Behavior & Ethology (AREA)
- Public Health (AREA)
- Veterinary Medicine (AREA)
- Polymers & Plastics (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Molecular Biology (AREA)
- Organic Chemistry (AREA)
- Birds (AREA)
- Epidemiology (AREA)
- Sustainable Development (AREA)
- Biochemistry (AREA)
- Engineering & Computer Science (AREA)
- Dermatology (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses an application of bletilla striata polysaccharide in preparing a product with a moisturizing effect, and relates to the technical field of plant extraction, wherein the preparation of the bletilla striata polysaccharide comprises the steps of heating and extracting a mixed solution of bletilla striata powder and water, and concentrating a supernatant of the extracted product to obtain colloidal bletilla striata polysaccharide; alcohol precipitation is carried out on the colloidal bletilla striata polysaccharide to obtain the bletilla striata polysaccharide; wherein the temperature of the heating extraction is 60-80 ℃ and the time is 1-8 h. Aiming at the moisturizing effect, the invention optimizes the extraction process parameters of the bletilla striata polysaccharide, improves the extraction rate and purity of the bletilla striata polysaccharide, and simultaneously ensures that the prepared bletilla striata polysaccharide has better moisture absorption rate and moisturizing rate.
Description
Technical Field
The invention relates to the technical field of plant extraction, in particular to application of bletilla striata polysaccharide in preparation of a product with a moisturizing effect.
Background
Moisture contained in human skin, which is reduced by an increase in age, temperature of the environment, and humidity, inevitably accelerates relaxation and aging of the skin. At present, the moisturizing skin care product has the defects of single moisturizing component, potential toxic and side effects and the like, and the research and the discovery of new substances with moisturizing effect are still key.
In view of this, the present invention has been made.
Disclosure of Invention
The invention aims to provide an application of bletilla striata polysaccharide in preparing a product with a moisturizing effect.
The invention is realized in the following way:
in a first aspect, an embodiment of the present invention provides an application of a bletilla striata polysaccharide in preparing a product with a moisturizing effect, where the extraction method of the bletilla striata polysaccharide includes: heating and extracting the mixed solution of the bletilla striata powder and water, and concentrating the supernatant of the extracted product to obtain colloidal bletilla striata polysaccharide; alcohol precipitation is carried out on the colloidal bletilla striata polysaccharide to obtain the bletilla striata polysaccharide; wherein the temperature of the heating extraction is 60-80 ℃ and the time is 1-8 h.
In a second aspect, an embodiment of the present invention provides a bletilla striata polysaccharide, which is extracted by the extraction method described in the foregoing embodiment.
In a third aspect, embodiments of the present invention provide a moisturizing product comprising: the bletilla striata polysaccharide of the previous embodiment or the bletilla striata polysaccharide obtained by extraction of the previous embodiment.
The invention has the following beneficial effects:
according to the invention, aiming at the moisturizing effect, the extraction process parameters of the bletilla striata polysaccharide are optimized, the starch gelatinization of the starch in the bletilla striata is avoided due to overhigh temperature by improving the temperature and time of heating extraction, the extraction rate and purity of the bletilla striata polysaccharide are improved, and compared with other natural polysaccharide moisturizers, the bletilla striata polysaccharide prepared by the method has better moisture absorption rate and moisturizing rate.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention more clear, the technical solutions of the embodiments of the present invention will be clearly and completely described below. The specific conditions are not noted in the examples and are carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or apparatus used were conventional products commercially available without the manufacturer's attention.
The Bletilla striata is a dry tuber of the perennial herb Bletilla striata of orchidaceae, namely Bletilla striata (thunder.) Reichb.f., is one of traditional Chinese medicinal materials, has the effects of promoting granulation, stopping bleeding, eliminating phlegm, lung diseases, treating chronic gastric ulcer and the like, and the Bletilla striata polysaccharide is an active compound which has important medicinal value, the main component is glucomannan, and the mannose and glucose ratio is about 4:1, has the advantages of high viscosity, good biocompatibility, easy degradation and the like, and can be used as a natural thickening agent and an emulsion stabilizer.
The extraction efficiency, purity and moisturizing effect of the existing bletilla striata polysaccharide are all to be improved. The inventor researches find that the bletilla striata polysaccharide extracted under a specific process has high moisture retention rate and moisture retention efficacy under the condition of good polysaccharide extraction rate and purity, and can be widely applied to daily skin moisture retention, including daily skin moisture retention of face, hands and body.
Specifically, the embodiment of the invention provides an application of bletilla striata polysaccharide in preparing a product with a moisturizing effect, and the extraction method of the bletilla striata polysaccharide comprises the following steps: heating and extracting the mixed solution of the bletilla striata powder and water, and concentrating the supernatant of the extracted product to obtain colloidal bletilla striata polysaccharide; alcohol precipitation is carried out on the colloidal bletilla striata polysaccharide to obtain the bletilla striata polysaccharide; wherein the temperature of the heating extraction is 60-80 ℃ and the time is 1-8 h.
The applicant discovers through a series of creative labor that by improving the temperature and time of heating extraction, starch gelatinization in the bletilla striata can be prevented from being accelerated due to overhigh temperature, the extraction rate and purity of the bletilla striata polysaccharide are improved, and compared with other natural polysaccharide moisturizers, the bletilla striata polysaccharide prepared by the method has better bletilla striata extraction rate, moisture absorption rate and moisture retention rate; under the condition of ensuring the extraction rate of polysaccharide, the high-purity bletilla striata polysaccharide has higher active ingredients, so that the moisturizing effect is promoted, the reaction temperature and the reaction time are higher, the feed-liquid ratio is increased, the increase of the extraction rate, the purity and the moisturizing effect is not greatly influenced, and the cost is increased.
The "bletilla striata powder" herein refers to a powder of bletilla striata tubers.
Specifically, the temperature of the heat extraction may be in a range between any one or any two of 60 ℃, 62 ℃, 64 ℃, 66 ℃, 68 ℃, 70 ℃, 72 ℃, 74 ℃, 76 ℃, 78 ℃,80 ℃; the heating extraction time can be any one or any two of 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 4.5h, 5h, 5.5h, 6h, 6.5h, 7h, 7.5h and 8h.
In some embodiments, the temperature of the heated extraction is: the solubility of the bletilla striata polysaccharide in the aqueous solution can be increased by increasing the extraction temperature to 65-80 ℃.
In some embodiments, the temperature of the heated extraction is: 65-78 ℃. The temperature range can better avoid starch gelatinization, thereby further improving the extraction rate, purity and moisturizing effect of the bletilla striata polysaccharide.
In some embodiments, the time of the heat extraction is: and 1-4 h.
In some embodiments, the time of the heat extraction is: and 2-4 h, and heating for a proper time to promote the dissolution of the bletilla striata polysaccharide.
In some embodiments, the pressure of the heated extraction is atmospheric pressure. The normal pressure is one atmosphere, which is the pressure of the gas generated by the atmosphere in normal life, and can be approximately regarded as one standard atmosphere, namely 100KPa or 0.1MPa. The process can ensure the dissolution of most of polysaccharide in the bletilla striata powder particles under normal pressure, is safer than pressurizing, has low requirements on equipment, and is easier to operate.
In some embodiments, the number of heat extractions is at least 1 or more.
In some embodiments, the number of heat extractions is 2-4. The number of times can be specifically 2 times, 3 times or 4 times, and the extraction times can be increased, so that the polysaccharide in the bletilla striata powder can be fully dissolved into water, and more water-soluble polysaccharide can be obtained as much as possible.
In some embodiments, the heated extraction feed ratio is 1: (10-30); wherein the feed liquid ratio is a volume ratio. The feed liquid ratio may specifically be in a range between any one or any two of 1:10, 1:12, 1:14, 1:16, 1:18, 1:20, 1:22, 1:24, 1:26, 1:28 and 1:30. The bletilla striata powder has strong water absorbability, and can promote the dissolution of polysaccharide in the powder and increase the extraction rate. The ratio of feed liquid is low, and the bletilla striata powder cannot be fully swelled, so that the powder is lump, and the extraction rate is seriously reduced; the higher feed-liquid ratio increases the dissolution of more water-soluble non-sugar substances on one hand, increases the volume of a reaction system on the other hand, and has higher requirements on equipment.
In some embodiments, the feed to liquid ratio is 1: (10-20), the feed-liquid ratio can increase the dissolution rate of polysaccharide.
In some embodiments, the step of alcohol precipitation comprises: adding the colloidal bletilla striata polysaccharide into an ethanol solution, and collecting precipitate.
In some embodiments, the concentration of the ethanol solution is greater than or equal to 95%. The ethanol with high concentration can promote the formation of precipitate of bletilla polysaccharide and reduce the consumption of ethanol solution. The concentration of the ethanol solution may specifically be in a range between any one or any two of 95%, 96%, 97%, 98%, 99%, and 100%. The "%" refers to volume percent.
In some embodiments, the volume ratio of the colloidal bletilla striata polysaccharide to the ethanol solution is 1: (1-4); the volume ratio may specifically be in a range between any one or any two of 1:1, 1:2, 1:3, and 1:4.
In some embodiments, the volume ratio of the colloidal bletilla striata polysaccharide to the ethanol solution is 1:4. the ethanol with the volume of 4 times can lead all the bletilla striata polysaccharide in the water extract to form precipitation, and can remove other small molecular compounds to improve the purity of the polysaccharide.
In some embodiments, the time of the alcohol precipitation is: 8-12h.
In some embodiments, the ethanol solution is a pre-chilled ethanol solution.
In some embodiments, pre-cooling refers to pre-cooling to 2-8deg.C, which can rapidly precipitate polysaccharide while removing other small molecule compounds.
In some embodiments, the alcohol precipitation further comprises drying the collected precipitate to obtain the bletilla striata polysaccharide.
In some embodiments, the extraction method further comprises: separating and purifying the bletilla striata polysaccharide;
in some embodiments, the separation and purification comprises: preparing bletilla striata polysaccharide solution from the bletilla striata polysaccharide obtained after alcohol precipitation, and obtaining purified bletilla striata polysaccharide after anion column chromatography;
in some embodiments, before performing the anion column chromatography, the separating and purifying further comprises centrifuging the bletilla striata polysaccharide solution, and taking a supernatant after centrifugation for anion column chromatography;
in some embodiments, the anion chromatography column comprises a DE-252 anion column;
in some embodiments, the concentration of the bletilla striata polysaccharide solution is 40-60 mg/mL, and the solvent is water. Specifically, the concentration of the bletilla striata polysaccharide solution can be any one or any range between two of 40mg/mL, 42mg/mL, 44mg/mL, 46mg/mL, 48mg/mL, 50mg/mL, 52mg/mL, 54mg/mL, 56mg/mL, 58mg/mL and 60 mg/mL.
In some embodiments, the eluent employed for the anion column chromatography is: naCl solutions with different gradients.
In some embodiments, the concentration of the NaCl solution at the different gradients comprises: 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL.
In some embodiments, the separation and purification further comprises: concentrating the eluted component obtained after anion column chromatography, performing alcohol precipitation (the alcohol precipitation step is the same as that of any embodiment), and collecting precipitate to obtain final bletilla striata polysaccharide.
Optionally, the product comprises: skin care product and/or care product, wherein the skin care product comprises rhizoma Bletillae facial cream, hand cream, lotion, hand leave-on gel, etc.
In some embodiments, the polysaccharide extraction rate of the bletilla striata polysaccharide is any one or more than two of 23%, 24%, 26%, 28%, 30%, 32%, 34%, 36%, 38%, 40%, 42%.
In some embodiments, the purity of the bletilla striata polysaccharide is 65%, 66%, 67%, 68%, 69%, 70%, 71%, 72%, 73% or more than a range between any two.
In some embodiments, the bletilla striata polysaccharide has a moisture retention rate in a range of between any one or more than any two of 36%, 37%, 38%, 39%, 40%.
In some embodiments, the bletilla striata polysaccharide has a moisture retention rate of any one or more than two of 99%, 99.1%, 99.2%, 99.3%, 99.4%, 99.5%, 99.6%, 99.7%, 99.8%, 99.9% at 43% RH.
In some embodiments, the bletilla striata polysaccharide has a moisture retention rate of any one or more than two of 95%, 96%, 97%, 98%, 99%, 100%, 101%, 102%, 103%, 104%, 105%, 106%, 107%, 108%, 109% at an RH of 81%.
On the other hand, the embodiment of the invention also provides a bletilla striata polysaccharide, which is extracted by the extraction method in any embodiment.
In addition, the embodiment of the invention also provides a moisturizing product, which comprises the bletilla striata polysaccharide in any embodiment or the bletilla striata polysaccharide extracted by the extraction method in any embodiment.
The features and capabilities of the present invention are described in further detail below in connection with the examples.
Example 1
An extraction method of bletilla striata polysaccharide comprises the following steps:
(1) Pulverizing rhizoma Bletillae tuber to obtain rhizoma Bletillae tuber powder, sieving with 200 mesh sieve, adding 20 times of distilled water, swelling, homogenizing, extracting at 80deg.C for 4 hr, filtering, adding 20 times of distilled water into the residue, repeating the extraction steps, extracting twice, mixing the supernatants, and concentrating to obtain rhizoma Bletillae polysaccharide gum.
(2) Slowly adding 1 time of 95% ethanol precooled to 4 ℃ into the bletilla striata polysaccharide gum in the step (1), placing the mixture in a refrigerator at 4 ℃ overnight, collecting precipitate, and freeze-drying the precipitate in a freeze dryer to obtain the bletilla striata crude polysaccharide.
(3) Preparing the crude polysaccharide of the bletilla striata in the step (2) into a solution with the concentration of 50mg/mL in advance, centrifuging, absorbing supernatant, separating and purifying by using DE-252 anion column chromatography, eluting sodium chloride with the concentration of 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL, eluting the solution with the volume of about 1-2 times of the column volume, collecting polysaccharide eluents under sodium chloride solutions with different concentrations, concentrating, precipitating with 95% ethanol precooled (4 ℃), refrigerating overnight at 4 ℃, collecting precipitate, and freeze-drying.
Example 2
An extraction method of bletilla striata polysaccharide comprises the following steps:
(1) Pulverizing rhizoma Bletillae tuber to obtain rhizoma Bletillae tuber powder, adding 20 times of distilled water, homogenizing, extracting at 80deg.C for 2 hr, filtering, adding 20 times of distilled water into the residue, repeating the extraction steps, extracting twice, mixing the supernatants, and concentrating to obtain rhizoma Bletillae polysaccharide gum.
(2) Slowly adding 1 time volume of pre-cooled (4 ℃) 95% ethanol into the bletilla striata polysaccharide gum in the step (1), placing the mixture in a refrigerator at 4 ℃ overnight, collecting precipitate, and freeze-drying the precipitate in a freeze dryer to obtain the bletilla striata crude polysaccharide.
(3) Preparing the crude polysaccharide of the bletilla striata in the step (2) into a solution with the concentration of 50mg/mL in advance, centrifuging, absorbing supernatant, separating and purifying by using DE-252 anion column chromatography, eluting sodium chloride with the concentration of 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL, eluting the solution with the volume of about 1-2 times of the column volume, collecting polysaccharide eluents under sodium chloride solutions with different concentrations, concentrating, precipitating with 95% ethanol precooled (4 ℃), refrigerating overnight at 4 ℃, collecting precipitate, and freeze-drying.
Example 3
An extraction method of bletilla striata polysaccharide comprises the following steps:
(1) Pulverizing rhizoma Bletillae tuber to obtain rhizoma Bletillae tuber powder, adding 20 times of distilled water, homogenizing, extracting at 60deg.C for 4 hr, filtering, adding 20 times of distilled water, repeating the extraction steps, extracting twice, mixing the supernatants, and concentrating to obtain rhizoma Bletillae polysaccharide gum.
(2) Slowly adding 1 time volume of pre-cooled (4 ℃) 95% ethanol into the bletilla striata polysaccharide gum in the step (1), placing the mixture in a refrigerator at 4 ℃ overnight, collecting precipitate, and freeze-drying the precipitate in a freeze dryer to obtain the bletilla striata crude polysaccharide.
(3) Preparing the crude polysaccharide of the bletilla striata in the step (2) into a solution with the concentration of 50mg/mL in advance, centrifuging, absorbing supernatant, separating and purifying by using DE-252 anion column chromatography, eluting sodium chloride with the concentration of 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL, eluting the solution with the volume of about 1-2 times of the column volume, collecting polysaccharide eluents under sodium chloride solutions with different concentrations, concentrating, precipitating with 95% ethanol precooled (4 ℃), refrigerating overnight at 4 ℃, collecting precipitate, and freeze-drying.
Example 4
An extraction method of bletilla striata polysaccharide comprises the following steps:
(1) Pulverizing rhizoma Bletillae tuber to obtain rhizoma Bletillae tuber powder, adding 20 times of distilled water, swelling, homogenizing, extracting at 60deg.C for 2 hr, filtering, adding 20 times of distilled water, repeating the extraction steps, extracting twice, mixing the supernatants, and concentrating to obtain rhizoma Bletillae polysaccharide gum.
(2) Slowly adding 1 time volume of pre-cooled (4 ℃) 95% ethanol into the bletilla striata polysaccharide gum in the step (1), placing the mixture in a refrigerator at 4 ℃ overnight, collecting precipitate, and freeze-drying the precipitate in a freeze dryer to obtain the bletilla striata crude polysaccharide.
(3) Preparing the crude polysaccharide of the bletilla striata in the step (2) into a solution with the concentration of 50mg/mL in advance, centrifuging, absorbing supernatant, separating and purifying by using DE-252 anion column chromatography, eluting sodium chloride with the concentration of 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL, eluting the solution with the volume of about 1-2 times of the column volume, collecting polysaccharide eluents under sodium chloride solutions with different concentrations, concentrating, precipitating with 95% ethanol precooled (4 ℃), refrigerating overnight at 4 ℃, collecting precipitate, and freeze-drying.
Example 5
An extraction method of bletilla striata polysaccharide comprises the following steps:
(1) Pulverizing rhizoma Bletillae tuber to obtain rhizoma Bletillae tuber powder, adding 10 times of distilled water, homogenizing, extracting at 80deg.C for 2 hr, filtering, adding 10 times of distilled water into the residue, repeating the extraction steps, extracting twice, mixing the supernatants, and concentrating to obtain rhizoma Bletillae polysaccharide gum.
(2) Slowly adding 1 time volume of pre-cooled (4 ℃) 95% ethanol into the bletilla striata polysaccharide gum in the step (1), placing the mixture in a refrigerator at 4 ℃ overnight, collecting precipitate, and freeze-drying the precipitate in a freeze dryer to obtain the bletilla striata crude polysaccharide.
(3) Preparing the crude polysaccharide of the bletilla striata in the step (2) into a solution with the concentration of 50mg/mL in advance, centrifuging, absorbing supernatant, separating and purifying by using DE-252 anion column chromatography, eluting sodium chloride with the concentration of 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL, eluting the solution with the volume of about 1-2 times of the column volume, collecting polysaccharide eluents under sodium chloride solutions with different concentrations, concentrating, precipitating with 95% ethanol precooled (4 ℃), refrigerating overnight at 4 ℃, collecting precipitate, and freeze-drying.
Example 6
An extraction method of bletilla striata polysaccharide comprises the following steps:
(1) Pulverizing rhizoma Bletillae tuber to obtain rhizoma Bletillae tuber powder, adding 10 times of distilled water, homogenizing, extracting at 80deg.C for 4 hr, filtering, adding 10 times of distilled water into the residue, repeating the extraction steps, extracting twice, mixing the supernatants, and concentrating to obtain rhizoma Bletillae polysaccharide gum.
(2) Slowly adding 1 time volume of pre-cooled (4 ℃) 95% ethanol into the bletilla striata polysaccharide gum in the step (1), placing the mixture in a refrigerator at 4 ℃ overnight, collecting precipitate, and freeze-drying the precipitate in a freeze dryer to obtain the bletilla striata crude polysaccharide.
(3) Preparing the crude polysaccharide of the bletilla striata in the step (2) into a solution with the concentration of 50mg/mL in advance, centrifuging, absorbing supernatant, separating and purifying by using DE-252 anion column chromatography, eluting sodium chloride with the concentration of 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL, eluting the solution with the volume of about 1-2 times of the column volume, collecting polysaccharide eluents under sodium chloride solutions with different concentrations, concentrating, precipitating with 95% ethanol precooled (4 ℃), refrigerating overnight at 4 ℃, collecting precipitate, and freeze-drying.
Example 7
An extraction method of bletilla striata polysaccharide comprises the following steps:
(1) Pulverizing rhizoma Bletillae tuber to obtain rhizoma Bletillae tuber powder, adding 10 times of distilled water, homogenizing, extracting at 60deg.C for 4 hr, filtering, adding 10 times of distilled water into the residue, repeating the extraction steps, extracting twice, mixing the supernatants, and concentrating to obtain rhizoma Bletillae polysaccharide gum.
(2) Slowly adding 1 time volume of pre-cooled (4 ℃) 95% ethanol into the bletilla striata polysaccharide gum in the step (1), placing the mixture in a refrigerator at 4 ℃ overnight, collecting precipitate, and freeze-drying the precipitate in a freeze dryer to obtain the bletilla striata crude polysaccharide.
(3) Preparing the crude polysaccharide of the bletilla striata in the step (2) into a solution with the concentration of 50mg/mL in advance, centrifuging, absorbing supernatant, separating and purifying by using DE-252 anion column chromatography, eluting sodium chloride with the concentration of 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL, eluting the solution with the volume of about 1-2 times of the column volume, collecting polysaccharide eluents under sodium chloride solutions with different concentrations, concentrating, precipitating with 95% ethanol precooled (4 ℃), refrigerating overnight at 4 ℃, collecting precipitate, and freeze-drying.
Example 8
An extraction method of bletilla striata polysaccharide comprises the following steps:
(1) Pulverizing rhizoma Bletillae tuber to obtain rhizoma Bletillae tuber powder, adding 10 times of distilled water, swelling, homogenizing, extracting at 60deg.C for 2 hr, filtering, adding 10 times of distilled water, repeating the extraction steps, extracting twice, mixing the supernatants, and concentrating to obtain rhizoma Bletillae polysaccharide gum.
(2) Slowly adding 4 times of pre-cooled (4 ℃) 95% ethanol into the bletilla striata polysaccharide gum in the step (1), placing the mixture in a refrigerator at 4 ℃ overnight, collecting precipitate, and freeze-drying the precipitate in a freeze dryer to obtain the bletilla striata crude polysaccharide.
(3) Preparing the crude polysaccharide of the bletilla striata in the step (2) into a solution with the concentration of 50mg/mL in advance, centrifuging, absorbing supernatant, separating and purifying by using DE-252 anion column chromatography, eluting sodium chloride with the concentration of 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL, eluting the solution with the volume of about 1-2 times of the column volume, collecting polysaccharide eluents under sodium chloride solutions with different concentrations, concentrating, precipitating with 95% ethanol precooled (4 ℃), refrigerating overnight at 4 ℃, collecting precipitate, and freeze-drying.
Example 9
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 70 ℃.
Example 10
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 70 ℃ and the time is 2 hours.
Example 11
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 70 ℃ and the time is 6 hours.
Example 12
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 75 ℃ and the time is 2 hours.
Example 13
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 75 ℃ and the time is 4 hours.
Example 14
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 75 ℃ and the time is 6 hours.
Example 15
A method for extracting bletilla striata polysaccharide is substantially the same as in example 1, except that the heating extraction in step (1) is performed in a vacuum distillation tank.
Example 16
An extraction method of bletilla striata polysaccharide is similar to that of example 1, except that the pre-cooled 95% ethanol is replaced by the normal-temperature 95% ethanol in the step (2).
Example 17
An extraction method of bletilla striata polysaccharide is similar to that of example 1, except that pre-cooled ethanol is adopted in step (2) with a concentration of 90%.
Example 18
The extraction method of bletilla striata polysaccharide is basically the same as that of the embodiment 1, except that the feed liquid ratio in the step (1) is as follows: 1:15.
Example 19
The extraction method of bletilla striata polysaccharide is basically the same as that of the embodiment 1, except that the feed liquid ratio in the step (1) is as follows: 1:30.
Comparative example 1
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 50 ℃ and the time is 2 hours.
Comparative example 2
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 50 ℃ and the time is 4 hours.
Comparative example 3
A method for extracting bletilla striata polysaccharide is similar to that of example 1, except that the heating extraction temperature of step (1) is 50 ℃ and the time is 6 hours.
Test example 1
1. The polysaccharide extraction yield and purity of examples 1 to 8 were verified.
Experimental procedure
Crude polysaccharide extraction (%) = extract dry weight (g)/bletilla tuber powder (g); purity (%) refers to the milligrams of sugar contained in 1g of extract, and the specific implementation steps include: weighing 50mg of glucose which is dried to constant weight at 105 ℃, adding 500 mL of distilled water to prepare 0.1mg/mL of standard solution, diluting the distilled water to 0,0.02,0.04,0.06,0.08 and 0.1mg/mL, then adding 300 mu L of 6% phenol and 1.5mL of sulfuric acid respectively, shaking uniformly, standing for 10 minutes, detecting absorbance at 490nm, and drawing a standard curve by taking glucose content as an abscissa and OD value as an ordinate. The sample was prepared at 1mg/mL, the above procedure was repeated, absorbance was measured at 490nm, and the total sugar content of the sample was calculated by taking the standard curve.
Experimental results
TABLE 1 extraction yield and purity of polysaccharide
| Polysaccharide extraction yield (%) | Purity (%) | |
| Example 1 | 42.39 | 73.79 |
| Example 2 | 40.42 | 71.46 |
| Example 3 | 32.18 | 72.89 |
| Example 4 | 35.71 | 71.01 |
| Example 5 | 26.79 | 69.03 |
| Example 6 | 30.57 | 70.18 |
| Example 7 | 25.96 | 68.12 |
| Example 8 | 23.47 | 65.91 |
2. Measurement of moisturizing Property of moisturizer.
Measurement of moisture absorption Rate: the bletilla striata polysaccharide (examples 1 to 19 and comparative examples 1 to 3), glycerin and chitosan were weighed 500mg each, and then placed in a closed environment with a Relative Humidity (RH) of 43% and 81% for moisture absorption effect comparison, and after 48 hours, the weight of the three types of moisture absorbents after moisture absorption was weighed and recorded. Moisture absorption rate (X) = (W1-W0) ×100/W0, W0 and W1 represent the weight (g) of the humectant before and after moisture absorption, respectively.
Measurement of moisture retention: bletilla striata polysaccharide (examples 1-19 and comparative examples 1-3), glycerol, and chitosan were prepared into solutions of 1.0%, 5.0%, and 1.0%, respectively, and then subjected to Relative Humidity (RH)
The moisture absorption effect was compared in a closed environment of 43% and 81%, and the weight of the three types of moisture absorbents after moisture absorption was weighed and recorded after 48 hours. Moisture retention (%) =h1×100/H0, H1 and H0 represent the weight (g) of the aqueous solution before and after 48H of standing, respectively.
TABLE 2 moisture absorption and moisture retention of moisturizer
The data show that the extraction rate of the bletilla striata polysaccharide humectant separated from the bletilla striata tuber water extract is 42.39%, and the moisture retention performance of the bletilla striata polysaccharide humectant is better than that of glycerol and chitosan.
The above description is only of the preferred embodiments of the present invention and is not intended to limit the present invention, but various modifications and variations can be made to the present invention by those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. The application of the bletilla striata polysaccharide in preparing a product with moisturizing effect is characterized in that the extraction method of the bletilla striata polysaccharide comprises the following steps:
heating and extracting the mixed solution of the bletilla striata powder and water, and concentrating the supernatant of the extracted product to obtain colloidal bletilla striata polysaccharide;
alcohol precipitation is carried out on the colloidal bletilla striata polysaccharide to obtain the bletilla striata polysaccharide;
wherein the temperature of the heating extraction is 60-80 ℃ and the time is 1-8 h.
2. The use according to claim 1, wherein the temperature of the heat extraction is: 65-80 ℃;
preferably, the temperature of the heat extraction is: 65-78 ℃;
preferably, the time of the heat extraction is: 1-4 h;
preferably, the time of the heat extraction is: 2-4 h;
preferably, the pressure of the heating extraction is normal pressure.
3. The use according to claim 1, wherein the number of heat extractions is at least 1 or more than 1;
preferably, the number of times of the heat extraction is 2 to 4.
4. The use according to claim 3, wherein the ratio of feed liquid extracted by heating is 1: (10-30); wherein the feed liquid ratio is a volume ratio;
preferably, the feed liquid ratio is 1: (10-20).
5. The use according to any one of claims 1 to 4, wherein the step of alcohol precipitation comprises: adding the colloidal bletilla striata polysaccharide into an ethanol solution, and collecting precipitate.
6. The use according to claim 5, wherein the concentration of the ethanol solution is greater than or equal to 95%;
preferably, when alcohol precipitation is performed, the volume ratio of the colloidal bletilla striata polysaccharide to the ethanol solution is 1: (1-4);
preferably, the volume ratio of the colloidal bletilla striata polysaccharide to the ethanol solution is 1:3, a step of;
preferably, the time of the alcohol precipitation is: 4-12 h;
preferably, the ethanol solution is a precooled ethanol solution;
preferably, the pre-cooling refers to pre-cooling to 4-8 ℃;
preferably, the alcohol precipitation further comprises drying the collected precipitate to obtain the bletilla striata polysaccharide.
7. The use according to any one of claims 1 to 4, wherein the extraction method further comprises: separating and purifying the bletilla striata polysaccharide;
preferably, the separation and purification comprises: preparing bletilla striata polysaccharide solution from the bletilla striata polysaccharide obtained after alcohol precipitation, and obtaining purified bletilla striata polysaccharide after anion column chromatography;
preferably, before the anion column chromatography, the separation and purification further comprises centrifuging the bletilla striata polysaccharide solution, and taking supernatant after centrifugation for anion column chromatography;
preferably, the anion column comprises a DE-252 anion column;
preferably, the concentration of the bletilla striata polysaccharide solution is 40-60 mg/mL, and the solvent is water;
preferably, the eluent used for anion column chromatography is: naCl solutions with different gradients;
preferably, the concentration of the NaCl solution of different gradients comprises: 0mol/mL, 0.5mol/mL, 1mol/mL and 2mol/mL;
preferably, the separation and purification further comprises: concentrating the eluted component obtained after anion column chromatography, carrying out alcohol precipitation after concentrating, and collecting precipitate to obtain the final bletilla striata polysaccharide.
8. The use according to any one of claims 1 to 4, wherein the product comprises: skin care and/or maintenance products;
preferably, the skin care product comprises: any one of face cream, hand cream, lotion and hand leave-on gel.
9. A bletilla striata polysaccharide, characterized in that it is extracted by the extraction method according to any one of claims 1 to 8.
10. A moisturizing product, characterized in that it comprises the bletilla striata polysaccharide of claim 9 or obtained by extraction according to any one of the extraction methods of claims 1 to 8.
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| CN113354750A (en) * | 2021-05-31 | 2021-09-07 | 西安绿天生物技术有限公司 | Extraction method and application of bletilla striata polysaccharide with moisturizing effect |
| CN114106212A (en) * | 2021-11-08 | 2022-03-01 | 四川丽妍工坊生物科技有限公司 | Bletilla ochracea polysaccharide and preparation method and application thereof |
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| CN101899174A (en) * | 2010-08-11 | 2010-12-01 | 珈侬生化科技(中国)有限公司 | Bletilla polysaccharide compound serving as cosmetic raw material and preparation method thereof |
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