CN111196864A - Dendrobium nobile polysaccharide with moisturizing effect and preparation method and application thereof - Google Patents
Dendrobium nobile polysaccharide with moisturizing effect and preparation method and application thereof Download PDFInfo
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- A61K36/18—Magnoliophyta (angiosperms)
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Abstract
The application relates to dendrobium nobile polysaccharide in the technical field of natural medicine extraction, which comprises two monosaccharides of D-glucuronic acid and D-galactose, wherein the two monosaccharides are in a molar ratio: 0.5-5: 1; the molecular weight range of the dendrobium nobile polysaccharide is as follows: 2000-3000 Da; the dendrobium nobile lindl polysaccharide extracted by the invention has obvious moisturizing effect and can be applied to skin-care and beauty-care products.
Description
Technical Field
The invention belongs to the technical field of natural medicine extraction, and particularly relates to dendrobium nobile polysaccharide with a moisturizing effect, and a preparation method and application thereof.
Background
Dendrobium nobile (Dendrobium nobile Lindl.) also called flat yellow grass, Royle rhaponticum carthamoides, etc., is a Dendrobium plant of the family Orchidaceae, is a traditional famous and precious medicinal plant in China, is listed as the top quality in Shen nong Ben Cao Jing as early as possible, and is known as one of the nine major immortals grass. The medicinal part is fresh or dry stem, and has effects of nourishing yin, replenishing vital essence, improving gastrointestinal function, reducing weight and prolonging life. Modern pharmacological studies show that the main effective components of dendrobium nobile are alkaloids and polysaccharide compounds, so that the dendrobium nobile lindl has multiple effects of resisting tumor, resisting oxidation, resisting aging, enhancing immunity, regulating gastrointestinal motility, reducing blood sugar, reducing blood fat and the like, and the researches find that the alkaloids and the polysaccharide components in the dendrobium nobile lindl have the effects of resisting inflammation, inhibiting bacteria, whitening, moisturizing and the like on skin.
Polysaccharides are polymeric carbohydrate polymers composed of glycosidically bonded sugar chains and at least more than 10 monosaccharides, and all carbohydrates and derivatives thereof that meet the concept of polymer are called polysaccharides. Polysaccharides are also important in their very wide distribution in nature. Some are components constituting animal and plant cell walls, such as peptidoglycan and cellulose; some are nutrients for animal and plant storage, such as glycogen and starch; some have special biological activity, such as heparin in human body has anticoagulant effect, and polysaccharide in pneumococcal cell wall has antigen effect. Polysaccharides composed of the same type of monosaccharide are called homopolysaccharides, such as starch, cellulose and glycogen; polysaccharides composed of different monosaccharides are called heteropolysaccharides, and gum arabic is composed of pentose, galactose, and the like, and is diverse in chemical structure. The range is also extremely large in terms of molecular weight.
The dendrobium nobile polysaccharide is the main existing form of carbohydrate in dendrobium nobile, and the content of the dendrobium nobile polysaccharide is as high as about 10 percent of dry weight. The dendrobium nobile lindl polysaccharide has multiple functions of resisting tumor, blood coagulation, virus, aging, immunity and the like. The invention provides a dendrobium nobile polysaccharide ingredient with a definite structure, which has good moisturizing effect and can be used for skin care and beauty products.
Disclosure of Invention
The invention aims to provide dendrobium nobile polysaccharide with a moisturizing effect, which has the moisturizing effect and higher application value.
The invention provides dendrobium nobile polysaccharide which comprises two monosaccharides, namely D-glucuronic acid and D-galactose, wherein the two monosaccharides are in a molar ratio of: 0.5-5: 1; the molecular weight range of the dendrobium nobile polysaccharide is as follows: 2000 to 3000 Da.
Further, the dendrobium nobile lindl polysaccharide has the following two monosaccharide ratios in terms of molar ratio: 3: 1.
Further, the dendrobium nobile polysaccharide molecular structure is as follows:
the invention also aims to provide a preparation method of the dendrobium nobile polysaccharide, which comprises the following steps:
1) adding 10-20 times of 0.5mol/L NaOH solution into dendrobium nobile lindl, and stirring and extracting for 2 hours at 70 ℃; after cooling, adding 6mol/L HCl solution until the pH value of the mixed solution is 2-3, and centrifuging to obtain supernatant; concentrating the supernatant to 1 time of the weight of the dendrobium nobile raw material, adding 95% ethanol with 4 times of volume, standing for 8-12 hours, centrifuging and collecting precipitates to obtain dendrobium nobile crude polysaccharide;
2) adding 5-10 times of water by weight into the dendrobium nobile crude polysaccharide for dissolving, and respectively adding 0.5mol/LH into the dendrobium nobile crude polysaccharide in water bath at the temperature of 30 DEG C2O2And 4.0mol/L acetic acid; and after the reaction is ended, carrying out ultrafiltration treatment to obtain the dendrobium nobile lindl polysaccharide.
More specifically, the preparation method comprises the following steps: 1) adding 15 times of 0.5mol/L NaOH solution into the dendrobium nobile lindl, and stirring and extracting for 2 hours at 70 ℃; after cooling, 6mol/L HCl solution is added until the pH value of the mixed solution is 2.5; centrifuging to obtain supernatant; concentrating the supernatant to 1 weight time of the dendrobium nobile raw material, adding 4 volumes of 95% edible ethanol, standing for 10 hours, centrifuging and collecting precipitate to obtain dendrobium nobile crude polysaccharide;
2) dissolving dendrobium nobile lindl crude polysaccharide in 8 times of water by weight, and respectively adding 0.5mol/LH into the solution in water bath at the temperature of 30 DEG C2O2And 4.0mol/L acetic acid; and after the reaction is ended, carrying out ultrafiltration treatment to obtain the dendrobium nobile lindl polysaccharide.
The invention also aims to provide the application of the dendrobium nobile lindl polysaccharide in skin care products.
In particular, the skin care product has a moisturizing effect.
The dendrobium nobile polysaccharide is prepared by directly degrading dendrobium nobile medicinal materials in NaOH solution, regulating pH value, salting out to obtain crude polysaccharide, further degrading and purifying the dendrobium nobile crude polysaccharide in H2O2 solution, and finally performing ultrafiltration treatment to obtain the dendrobium nobile polysaccharide, wherein the dendrobium nobile polysaccharide is prepared by condensing two monosaccharides D-glucuronic acid and D-galactose according to the ratio of 0.5-5: 1.
Drawings
FIG. 1 is a HPGPC chromatogram of dendrobium stem polysaccharide in the invention;
FIG. 2 is an infrared absorption spectrum of dendrobium nobile polysaccharide in the invention.
Detailed Description
The following is further detailed by way of specific embodiments:
the materials and reagents used in the following examples are, unless otherwise specified, commonly available.
Example 1:
a preparation method of dendrobium nobile polysaccharide comprises the following steps: taking 1Kg of dendrobium nobile, adding 15L of 0.5mol/L NaOH solution, and stirring and extracting at 70 ℃ for 2 hours; after cooling, adding 6mol/L HCl solution to adjust the pH value to 2.5; centrifuging to obtain supernatant. Concentrating the supernatant to about 1L, adding 4L of 95% edible ethanol, standing for 10 hr, centrifuging, and collecting precipitate to obtain 208g of herba Dendrobii crude polysaccharide.
Dissolving the above crude polysaccharide 200g in 1.6L water, adding 0.5mol/L H into the solution in 30 deg.C water bath2O24.0mmol/L acetic acid; after the reaction was completed for 4 hours, 130g of polysaccharide was obtained by ultrafiltration. Detecting by high performance gel chromatography (HPGPC) with Sephax Mono GPC-10MP gel chromatography column (4.6mm 300mm, 5 μm); taking 0.1mol/L sodium chloride as a mobile phase; the flow rate is 0.5 mL/min; the column temperature is 30 ℃; the difference detector detects Dendrobium nobile polysaccharide (shown in figure 1), and its molecular weight is 2500 Da.
Taking a proper amount of 3mg of dendrobium nobile polysaccharide, adding 500mg of KBr powder, uniformly grinding, tabletting, and analyzing by an infrared spectrometer, wherein the infrared spectrum absorption is shown in figure 2.
15mg of the dendrobium nobile polysaccharide is taken and added with deuterated pyridine to be dissolved, and the 1H/13C-NMR data of the dendrobium nobile polysaccharide is shown in table 1 after the dendrobium nobile polysaccharide is analyzed by a nuclear magnetic resonance spectrometer.
TABLE 2 Dendrobium nobile polysaccharide 1H/13C-NMR spectrogram data and attribution
Example 2:
a method for preparing herba Dendrobii polysaccharide comprises collecting 1Kg herba Dendrobii, adding 20L 0.5mol/L NaOH solution, and extracting at 70 deg.C under stirring for 2 hr; after cooling, adding 6mol/L HCl solution to adjust the pH value to 2; centrifuging to obtain supernatant. Concentrating the supernatant to about 1L, adding 4L of 95% edible ethanol, standing for 12 hr, centrifuging, and collecting precipitate to obtain 210g of herba Dendrobii crude polysaccharide.
Dissolving the above crude polysaccharide 200g in water 2L, adding 0.5mol/L H in water bath at 30 deg.C2O24.0mmol/L acetic acid; after the reaction was completed for 4 hours, the reaction mixture was ultrafiltered to obtain 141g of polysaccharide. The dendrobium nobile lindl polysaccharide is detected by high performance gel chromatography (HPGPC) and has a molecular weight of 3000 Da.
Example 3:
a preparation method of dendrobium nobile polysaccharide comprises the following steps: taking 1Kg of dendrobium nobile, adding 10L of 0.5mol/L NaOH solution, and stirring and extracting at 70 ℃ for 2 hours; after cooling, adding 6mol/L HCl solution to adjust the pH value to 3; centrifuging to obtain supernatant. Concentrating the supernatant to about 1L, adding 4L of 95% edible ethanol, standing for 8 hr, centrifuging, and collecting precipitate to obtain 190g of crude herba Dendrobii polysaccharide.
Dissolving 150g of the crude polysaccharide in 0.75L of water, and adding 0.5mol/L H into the solution in 30 deg.C water bath2O24.0mmol/L acetic acid; after the reaction was terminated, the reaction was carried out for 4 hours, and then ultrafiltration treatment was carried out to obtain 90g of polysaccharide. The dendrobium nobile lindl polysaccharide is detected by high performance gel chromatography (HPGPC) and has a molecular weight of 2200 Da.
And (4) verifying a moisturizing experiment:
60 volunteers were collected and divided into 3 groups of 20 individuals, and skin moisture values were measured at different time periods before and after using the dendrobium nobile polysaccharides of examples 1 to 3. Before the experiment, all volunteers firstly wash the face with warm water, the average value of the moisture value of the face skin is measured (0min) after the skin is naturally dried, 0.1g of dendrobium nobile polysaccharide is dissolved in 10mL of purified water and then is uniformly coated on the face, the dendrobium nobile polysaccharide is washed off after 15min, the average value of the moisture value of the skin is measured (45min) after 30min and the average value of the moisture value of the skin is measured (75min) after 30min, and the measurement results are as follows:
TABLE 2 moisture value of skin before and after using the mask
TABLE 2 moisture value of skin before and after using the mask
| Grouping | | 45min | 75min | |
| 1 | 29％ | 70％ | 52％ | |
| 2 | 28％ | 68％ | 50％ | |
| 3 | 29％ | 69％ | 49％ |
The detection results show that the moisture value of the skin is greatly improved after the dendrobium nobile polysaccharide in the embodiments is used compared with that before the dendrobium nobile polysaccharide is used, and particularly, the dendrobium nobile polysaccharide in the embodiment 1 has the best moisturizing effect. Therefore, the dendrobium nobile lindl polysaccharide can increase the moisture value of the skin and has good moisturizing and hydrating effects.
Claims (6)
1. A dendrobium nobile polysaccharide is characterized in that: comprises two monosaccharides, namely D-glucuronic acid and D-galactose, wherein the ratio of the two monosaccharides is as follows in molar ratio: 0.5-5: 1; the molecular weight range of the dendrobium nobile polysaccharide is as follows: 2000 to 3000 Da.
2. The dendrobium nobile polysaccharide according to claim 1, characterized in that: the dendrobium nobile polysaccharide is characterized in that the dendrobium nobile polysaccharide has two monosaccharide ratios in terms of molar ratio: 3: 1.
3. The dendrobium nobile polysaccharide according to claim 2, characterized in that: the dendrobium nobile polysaccharide molecular structure is as follows:
4. the method for preparing dendrobium nobile lindl polysaccharide according to any one of claims 1 to 3, characterized in that: the preparation method comprises the following steps:
1) adding 10-20 times of 0.5mol/L NaOH solution into dendrobium nobile lindl, and stirring and extracting for 2 hours at 70 ℃; after cooling, adding 6mol/L HCl solution until the pH value of the mixed solution is 2-3, and centrifuging to obtain supernatant; concentrating the supernatant to 1 time of the weight of the dendrobium nobile raw material, adding 95% ethanol with 4 times of volume, standing for 8-12 hours, centrifuging and collecting precipitates to obtain dendrobium nobile crude polysaccharide;
2) adding 5-10 times of water by weight into the dendrobium nobile crude polysaccharide for dissolving, and respectively adding 0.5mol/LH into the dendrobium nobile crude polysaccharide in water bath at the temperature of 30 DEG C2O2And 4.0mol/L acetic acid; and after the reaction is ended, carrying out ultrafiltration treatment to obtain the dendrobium nobile lindl polysaccharide.
5. The use of dendrobium nobile lindl polysaccharide according to any one of claims 1 to 3 in skin care products.
6. The use according to claim 5, said skin care product having a moisturizing effect.
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Cited By (2)
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| CN113413329A (en) * | 2021-08-02 | 2021-09-21 | 遵义医科大学 | Dendrobium nobile polysaccharide herbal face cream and preparation method thereof |
| CN114469985A (en) * | 2020-10-23 | 2022-05-13 | 遵义医科大学 | Dendrobium stem medicinal composition and preparation method of antibacterial gel thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114469985A (en) * | 2020-10-23 | 2022-05-13 | 遵义医科大学 | Dendrobium stem medicinal composition and preparation method of antibacterial gel thereof |
| CN114469985B (en) * | 2020-10-23 | 2024-04-19 | 遵义医科大学 | Dendrobium nobile medicinal composition and preparation method of antibacterial gel thereof |
| CN113413329A (en) * | 2021-08-02 | 2021-09-21 | 遵义医科大学 | Dendrobium nobile polysaccharide herbal face cream and preparation method thereof |
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Effective date of registration: 20220615 Address after: 537000 Ma Lu Ling, Shihe Town, Fumian District, Yulin City, Guangxi Zhuang Autonomous Region Patentee after: Guangxi Shenli Pharmaceutical Co.,Ltd. Address before: 563000 No. 201, Dalian Road, Huichuan District, Zunyi City, Guizhou Province Patentee before: ZUNYI MEDICAL University |