Preparation method of medicinal liquor containing dendrobium officinale

Abstract

The invention discloses a preparation method of medicinal liquor containing dendrobium officinale, which is characterized in that an extraction solvent is prepared by using octyl and decyl glucoside and ethylene glycol monophenyl ether as components to replace a conventional organic solvent, so that the production cost is reduced while the extraction effect is enhanced; a deep eutectic solvent is prepared from N, N-dimethylglycine and tetradecyl hydroxypropyl phosphate betaine, and the problem that the extraction effect is poor due to the fact that conventional amino acid is poor in thermal stability and conventional betaine is high in thickening property is solved; by preparing the water-soluble stabilizer, the problem that the stability of the medicinal liquor cannot be effectively enhanced due to the fact that a conventional stabilizer cannot be completely fused with the liquor due to poor water solubility is solved.

Description

Technical Field

[0001] The invention belongs to the technical field of medicinal wine preparation, and particularly relates to a method for preparing medicinal wine containing dendrobium candidum. Background Art

[0002] Dendrobium officinale, belonging to the orchid family, is a precious plant resource that can be used as both medicine and food. It contains many beneficial ingredients such as astragalus substances and Dendrobium officinale polysaccharides. It has the effects of nourishing yin, tonifying the spleen and stomach, protecting the liver and promoting bile secretion, lowering blood sugar, inhibiting tumors, nourishing the skin and prolonging life. There are rich types of stilbene substances in Dendrobium officinale, with high content and strong biological activity. At present, the extraction methods of stilbene substances include traditional methods such as immersion method, percolation method, water extraction and decoction method, reflux extraction method and a new extraction method of tank assembly dynamic countercurrent method. The traditional methods have low extraction efficiency and high energy consumption, and the tank assembly dynamic countercurrent method generally uses ethanol and ethyl acetate as extraction solvents, both of which are volatile substances, and need to be heated to a higher temperature during extraction to improve the extraction effect. On the one hand, the solvent will evaporate and the extraction effect will be reduced. On the other hand, the higher temperature will also make other effective ingredients in Dendrobium officinale, such as Dendrobium officinale polysaccharides, less stable and decompose, weakening their efficacy. In addition, ethyl acetate will react due to acid-base treatment during the extraction process, which will produce impurities on the one hand and make ethyl acetate unable to be recycled on the other hand, increasing production costs.

[0003] Dendrobium officinale also contains rich Dendrobium officinale polysaccharides. Low eutectic solvents are a new type of solvents with the characteristics of simple preparation, low cost, low toxicity, good solubility and non-volatility. Amino acids and betaine are commonly used components in low eutectic solvents, but the former has the defect of poor thermal stability and is prone to decomposition and other reactions at high temperatures, which makes the stability of the low eutectic solvent worse and affects the extraction of Dendrobium officinale polysaccharides. The latter generally has a thickening effect, which will further increase the viscosity of the low eutectic solvent on the basis of its own high viscosity, resulting in poor extraction effect. Summary of the invention

[0004] The purpose of the present invention is to provide a method for preparing a medicinal wine containing dendrobium candidum.

[0005] In order to solve the above technical problems, the technical solution adopted by the present invention comprises the following steps: A method for preparing a medicinal wine containing dendrobium officinale, comprising the following specific steps: (1) Weigh the powder of Dendrobium officinale, add 8 to 10 times the weight of petroleum ether to degrease at 40 to 50°C, add 5 to 7 times the weight of the powder of Dendrobium officinale to an extractant a having wetting and dual surfactant properties, and then extract the powder using a tank-type tank assembly dynamic countercurrent method. After the extraction, separate the solid a and the extract, add a dilute sodium hydroxide solution to the extract and stir until the pH value of the aqueous phase is 7.01 to 7.03, separate the organic phase and recycle it, add dilute hydrochloric acid to the aqueous phase until the pH value is 5.0 to 5.4, stir well, let stand for 2 to 3 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain the Dendrobium officinale stilbene-like substance; (2) solid a is immersed in anhydrous ethanol, fully stirred, filtered and dried, then solid a and extractant b are mixed at a solid-liquid ratio of 1:24-26 g / ml, stirred at 70-80°C at a speed of 200-300 r / min for 55-65 min, filtered residue and filtrate, after the filtrate is cooled, 2-3 times the volume of anhydrous ethanol is added to the filtrate, precipitated at 2-4°C for 8-10 h, centrifuged at a speed of 3900-4100 r / min for 14-16 min, and dried to obtain Dendrobium officinale polysaccharide; (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.1-0.12, and then a nutrient solution of 2-3 times the mass of the filter residue is added, and fermented at 33-35° C. for 5-6 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 8-10 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substance obtained in step (1) and step (2) and the Dendrobium officinale polysaccharide are added to the fermentation liquid, and the mixture is uniformly stirred, sterilized and canned to obtain the Dendrobium officinale medicinal wine.

[0006] Furthermore, the preparation method of the extractant a in step (1) is: 0.3-0.5 parts of octyl decyl glucoside are added to 9-10 parts of ethylene glycol phenyl ether, followed by stirring at 40-50°C at a speed of 100-200 r / min for 10-12 minutes, and then cooling to obtain extractant a.

[0007] Furthermore, the tank group tank assembly dynamic countercurrent method in step (1) is specifically as follows: In the first extraction of the first tank of Dendrobium officinale powder, 5 to 7 times the mass of the extractant a is added, and in the second and third extractions, 5 to 7 times and 2 to 4 times the mass of the extractant a are added respectively; after the first tank extraction is completed, new Dendrobium officinale powder is added to the second tank, and the extract obtained from the second extraction in the first tank is added as the extractant to the second tank for the first extraction, and in the second extraction in the second tank, the extract obtained from the third extraction in the first tank is used as the extractant and the extractant a is supplemented to the same volume as the first extraction in the second tank, and 2 to 4 times the mass of the extractant a is added to the third extraction of Dendrobium officinale powder; the extraction method of the third tank is the same as that of the second tank, and the second extraction and the third extraction in the second tank are used as the first and second extractions in the third tank, respectively, and 3 to 5 times the mass of the extractant a is added to the third extraction of Dendrobium officinale powder; Among them, each extraction time is 60~80min, the extraction temperature is 65~70℃, and the stirring speed is 80~100r / min.

[0008] Furthermore, the preparation method of the extractant b in step (2) is: N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.0-3.2, and deionized water was added until the water content of the system was 30%-32%, and then the system was heated to 76-80°C and stirred continuously until a uniform and transparent solution was obtained, and then the extract b was obtained after cooling.

[0009] Furthermore, the nutrient solution in step (3) is: The product is obtained by uniformly mixing water, urea and glucose in a mass ratio of 1:0.02~0.04:0.02~0.04.

[0010] After the stilbene substances and polysaccharides in the Dendrobium candidum are added to the medicinal wine, on the one hand, the stilbene substances and polysaccharides will deteriorate due to oxidation reaction, which reduces the efficacy of the Dendrobium candidum medicinal wine. On the other hand, the solubility of the polysaccharide in the wine is low, and the polysaccharide will precipitate crystals in the wine due to changes in ambient temperature, which further affects the efficacy of the medicinal wine and also affects the taste and stability of the medicinal wine. Therefore, in order to enhance the stability of the Dendrobium candidum medicinal wine, a water-soluble stabilizer is provided as a supplement for the Dendrobium candidum medicinal wine. The specific preparation steps of the water-soluble stabilizer are: Add 2-3 parts of chicoric acid and 1-2 parts of salvianolic acid B to 30-40 parts of deionized water, and stir evenly at 20-30°C to obtain a water-soluble stabilizer; Among them, the mass ratio of Dendrobium officinale medicinal wine and water-soluble stabilizer is 1:0.05~0.07.

[0011] The beneficial effects of the present invention are: (1) The present invention prepares an extractant to replace conventional solvents as an extraction solvent for stilbenes in Dendrobium officinale. Compared with conventional extraction solvents such as ethyl acetate, ethylene glycol phenyl ether has low volatility and better permeability, and can more effectively extract stilbenes in Dendrobium officinale. On the other hand, ethylene glycol phenyl ether can be dissolved in sodium hydroxide solution but is insoluble in water and will not react with acid or alkali. The pH value in the alkali treatment step can be measured to determine whether the stilbenes have been completely converted into water-soluble salts. At the same time, after the conversion is completed, two liquid phases will be formed due to the poor water solubility of ethylene glycol phenyl ether. After the conversion is completed, ethylene glycol phenyl ether can be separated and removed, thereby avoiding the problem of ethyl acetate reacting with sodium hydroxide to produce impurities. At the same time, part of the extractant components can be recovered, thereby reducing production costs. (2) In order to further improve the extraction effect of stilbene substances, a wetting agent is used as one of the components of the extractant. The wetting agent can enhance the wetting effect of the extractant on the surface of Dendrobium officinale, promote the release and dissolution of stilbene substances, and achieve the purpose of improving the extraction effect. However, conventional wetting agents such as sodium dodecyl sulfate have the problems of poor stability and poor solubility in organic solvents. They are easily affected by conditions such as pH and then inactivated. Octyl decyl glucoside is a surfactant with both nonionic and anionic properties. It has excellent wettability and can effectively enhance the wetting properties of the extractant. It is also easily soluble in organic solvents and can form a uniform component with ethylene glycol phenyl ether, so the extraction effect will not be affected by uneven components. (3) The present invention uses a low eutectic solvent to extract Dendrobium officinale polysaccharides. Amino acids are common components of low eutectic solvents. N,N-dimethylglycine is also an amino acid. Compared with conventional amino acids such as glycine, it has better thermal stability and the viscosity of the low eutectic solvent formed is also lower. Dendrobium officinale polysaccharides can be better extracted at a higher temperature, which accelerates the extraction efficiency on the one hand and improves the extraction rate on the other hand. (4) Betaine is also a common component of low eutectic solvents. It has good penetration and wettability and can effectively extract Dendrobium polysaccharides. Compared with dodecyl dimethyl betaine, tetradecyl hydroxypropyl phosphate betaine does not have thickening properties and will not increase the viscosity of low eutectic solvents. Therefore, it is necessary to increase the extraction temperature to reduce the viscosity to achieve the purpose of improving the extraction effect. At the same time, it also has good solubility, which can further improve the extraction effect and reduce the extraction time. (5) The ingredients in the medicinal wine of Dendrobium candidum are easily affected by the environment and thus deteriorate and precipitate crystals, which affects the stability of the medicinal wine. Therefore, antioxidants are added to the medicinal wine to enhance its stability. Chicoric acid is a type of antioxidant, but during the research process, it was found that adding chicoric acid alone did not have a significant effect on enhancing the stability of the medicinal wine. Therefore, another antioxidant was added to it to enhance the stabilizer effect, but the effect of the combination of ferulic acid or caffeic acid was not obvious. The study found that the combination of tannic acid B and chicoric acid had a significant effect on the stability of the medicinal wine. The effect is very good, and it has a good synergistic effect. The reason may be that chicoric acid and salvianolic acid B can enhance each other's fusion with the Dendrobium Officinale Wine, making the components of the wine more uniform. On the one hand, it can better enhance the antioxidant properties of the Dendrobium Officinale Wine, and on the other hand, it can also ionize more hydrogen ions to hydrolyze the Dendrobium Officinale polysaccharides, thereby increasing the solubility of the Dendrobium Officinale polysaccharides in the wine, thereby achieving the purpose of enhancing the stability of the Dendrobium Officinale Wine and increasing the anti-inflammatory and immunity-enhancing effects of the Dendrobium Officinale Wine. DETAILED DESCRIPTION

[0012] The present invention will be further described in detail below in conjunction with the embodiments. Example 1

[0013] 0.4 parts of octyl glucoside were added to 9.5 parts of ethylene glycol phenyl ether, followed by stirring at 45°C and 150 r / min for 11 minutes, and then cooling to obtain extractant a.

[0014] The powder of Dendrobium officinale was weighed, and 9 times the mass of petroleum ether was added to perform degreasing treatment at 45°C. After the treatment, the powder of Dendrobium officinale was added to 6 times the mass of extractant a with wetting and dual surfactant properties, and then the extract was extracted by a tank-type tank assembly dynamic countercurrent method. After the extraction was completed, solid a and an extract were separated, and a dilute sodium hydroxide solution was added to the extract for stirring until the pH value of the aqueous phase was 7.02, and the organic phase was separated for recycling. At the same time, dilute hydrochloric acid was added to the aqueous phase to a pH value of 5.2, and the mixture was fully stirred and allowed to stand for 2.5 hours. The precipitate was separated by centrifugation, and the precipitate was washed with deionized water to obtain the Dendrobium officinale stilbene-like substance. Example 2

[0015] 0.3 parts of octyl decyl glucoside were added to 10 parts of ethylene glycol phenyl ether, followed by stirring at 200 r / min for 10 min at 40° C., and then cooling to obtain extractant a.

[0016] The powder of Dendrobium officinale was weighed, and 8 times the mass of petroleum ether was added to perform degreasing treatment at 50°C. After the treatment, the powder of Dendrobium officinale was added to 5 times the mass of the extractant a with wetting and dual surfactant properties, and then the extract was extracted by a tank-type tank assembly dynamic countercurrent method. After the extraction was completed, solid a and an extract were separated, and a dilute sodium hydroxide solution was added to the extract for stirring until the pH value of the aqueous phase was 7.01, and the organic phase was separated for recycling. At the same time, dilute hydrochloric acid was added to the aqueous phase to a pH value of 5.4, and the mixture was fully stirred and allowed to stand for 2 hours. The precipitate was separated by centrifugation, and the precipitate was washed with deionized water to obtain the Dendrobium officinale stilbene-like substance. Example 3

[0017] 0.5 parts of octyl glucoside were added to 9 parts of ethylene glycol phenyl ether, followed by stirring at 50° C. and 100 r / min for 12 min, and then cooling to obtain extractant a.

[0018] The powder of Dendrobium officinale was weighed, and petroleum ether with a mass of 10 times was added to perform degreasing treatment at 40°C. After the treatment, the powder of Dendrobium officinale was added to an extractant a with a wetting and dual surfactant property with a mass of 7 times, and then extracted by a tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and an extract were separated, and a dilute sodium hydroxide solution was added to the extract for stirring until the pH value of the aqueous phase was 7.03, and the organic phase was separated for recycling. At the same time, dilute hydrochloric acid was added to the aqueous phase to a pH value of 5.0, and the mixture was fully stirred and allowed to stand for 3 hours. The precipitate was separated by centrifugation, and the precipitate was washed with deionized water to obtain the Dendrobium officinale stilbene-like substance. Example 4

[0019] 0.4 parts of sodium dodecyl sulfate were added to 9.5 parts of ethylene glycol phenyl ether, followed by stirring at 45° C. and 150 r / min for 11 minutes, and then cooling to obtain extractant a.

[0020] The rest is the same as in Example 1. Example 5

[0021] 0.4 parts of octyl decyl glucoside were added to 9.5 parts of ethyl acetate, followed by stirring at 45°C and 150 r / min for 11 minutes, and then cooling to obtain extractant a.

[0022] The rest is the same as in Example 1. Example 6

[0023] 0.4 parts of octyl glucoside were added to 9.5 parts of ethylene glycol phenyl ether, followed by stirring at 30°C and 150 r / min for 11 minutes, and then cooling to obtain extractant a.

[0024] The rest is the same as in Example 1. Example 7

[0025] 0.4 parts of octyl glucoside were added to 9.5 parts of ethylene glycol phenyl ether, followed by stirring at 400 r / min for 11 minutes at 45°C, and then cooling to obtain extractant a.

[0026] The rest is the same as in Example 1. Example 8

[0027] The powder of Dendrobium officinale was weighed, and 9 times the mass of petroleum ether was added to perform degreasing treatment at 25°C. After the treatment, the powder of Dendrobium officinale was added to 6 times the mass of the extractant a with wetting and dual surfactant properties, and then the extract was extracted by a tank-type tank assembly dynamic countercurrent method. After the extraction was completed, solid a and an extract were separated, and a dilute sodium hydroxide solution was added to the extract for stirring until the pH value of the aqueous phase was 7.02, and the organic phase was separated for recycling. At the same time, dilute hydrochloric acid was added to the aqueous phase to a pH value of 5.2, and the mixture was fully stirred and allowed to stand for 2.5 hours. The precipitate was separated by centrifugation, and the precipitate was washed with deionized water to obtain the Dendrobium officinale stilbene-like substance.

[0028] The rest is the same as in Example 1. Example 9

[0029] The powder of Dendrobium officinale was weighed, and 9 times the weight of petroleum ether was added to perform degreasing treatment at 45°C. After the treatment, the powder of Dendrobium officinale was added to 3 times the weight of the extractant a with wetting and dual surfactant properties, and then the extract was extracted by a tank-type tank assembly dynamic countercurrent method. After the extraction was completed, solid a and an extract were separated, and a dilute sodium hydroxide solution was added to the extract for stirring until the pH value of the aqueous phase was 7.02, and the organic phase was separated for recycling. At the same time, dilute hydrochloric acid was added to the aqueous phase to a pH value of 5.2. After sufficient stirring, it was allowed to stand for 2.5 hours, and the precipitate was separated by centrifugation. The precipitate was washed with deionized water to obtain the Dendrobium officinale stilbene-like substance.

[0030] The rest is the same as in Example 1. Example 10

[0031] Weigh the Dendrobium officinale powder, add 9 times the mass of petroleum ether to degrease at 45°C, add the Dendrobium officinale powder to 6 times the mass of extractant a with wetting and dual surfactant properties, then extract at 67°C at a speed of 90r / min for 70min, separate the solid a and the extract after the extraction, add dilute sodium hydroxide solution to the extract and stir until the pH value of the aqueous phase is 7.02, separate the organic phase for recycling, add dilute hydrochloric acid to the aqueous phase to pH 5.2, stir well and let stand for 2.5h, centrifuge to obtain the precipitate, and wash with deionized water to obtain the Dendrobium officinale stilbene-like substance.

[0032] The rest is the same as in Example 1. Embodiment 11

[0033] The powder of Dendrobium officinale was weighed, and 9 times the mass of petroleum ether was added to perform degreasing treatment at 45°C. After the treatment, the powder of Dendrobium officinale was added to 6 times the mass of extractant a with wetting and dual surfactant properties, and then the extract was extracted by a tank-type tank assembly dynamic countercurrent method. After the extraction was completed, solid a and an extract were separated, and a dilute sodium hydroxide solution was added to the extract for stirring until the pH value of the aqueous phase was 8.0, and the organic phase was separated for recycling. At the same time, dilute hydrochloric acid was added to the aqueous phase to a pH value of 5.2. After sufficient stirring, it was allowed to stand for 2.5 hours, and the precipitate was separated by centrifugation. The precipitate was washed with deionized water to obtain the Dendrobium officinale stilbene-like substance.

[0034] The rest is the same as in Example 1. Example 12

[0035] The powder of Dendrobium officinale was weighed, and 9 times the mass of petroleum ether was added to perform degreasing treatment at 45°C. After the treatment, the powder of Dendrobium officinale was added to 6 times the mass of the extractant a with wetting and dual surfactant properties, and then the extract was extracted by a tank-type tank assembly dynamic countercurrent method. After the extraction was completed, solid a and an extract were separated, and a dilute sodium hydroxide solution was added to the extract to stir until the pH value of the aqueous phase was 7.02, and the organic phase was separated for recycling. At the same time, dilute hydrochloric acid was added to the aqueous phase to a pH value of 6.5. After sufficient stirring, it was allowed to stand for 2.5 hours, and the precipitate was separated by centrifugation. The precipitate was washed with deionized water to obtain the Dendrobium officinale stilbene-like substance.

[0036] The rest is the same as in Example 1. Embodiment 13

[0037] The powder of Dendrobium officinale was weighed, and 9 times the mass of petroleum ether was added to perform degreasing treatment at 45°C. After the treatment, the powder of Dendrobium officinale was added to 6 times the mass of extractant a with wetting and dual surfactant properties, and then the extract was extracted by a tank-type tank assembly dynamic countercurrent method. After the extraction was completed, solid a and an extract were separated, and a dilute sodium hydroxide solution was added to the extract for stirring until the pH value of the aqueous phase was 7.02, and the organic phase was separated for recycling. At the same time, dilute hydrochloric acid was added to the aqueous phase until the pH value was 5.2, and the mixture was fully stirred and allowed to stand for 1 hour. The precipitate was separated by centrifugation, and the precipitate was washed with deionized water to obtain the Dendrobium officinale stilbene-like substance.

[0038] Test 1: The mass M of the Dendrobium officinale powder and the mass m of the extracted Dendrobium officinale stilbene substances in Examples 1 to 13 were measured, and then the extraction rate of the Dendrobium officinale stilbene substances was calculated by the formula a=m / M. The specific data are shown in Table 1.

[0039] Table 1 Data table of extraction rate of stilbene substances in Examples 1 to 13 Implementation items a（%） Example 1 1.75 Example 2 1.72 Example 3 1.73 Example 4 1.51 Example 5 1.53 Example 6 1.65 Example 7 1.62 Example 8 1.67 Example 9 1.33 Example 10 1.41 Embodiment 11 1.59 Example 12 1.61 Embodiment 13 1.66 It can be seen from Table 1 that the extraction rate of stilbene substances in Examples 1 to 3 is the highest; in Examples 4 and 5, octyl decyl glucoside and ethylene glycol phenyl ether are replaced by sodium dodecyl sulfonate and ethyl acetate, respectively. Sodium dodecyl sulfonate has poor stability and low compatibility with ethylene glycol phenyl ether. Ethyl acetate is highly volatile and its content decreases due to volatilization during the extraction process, which affects the extraction effect of extractant a and further affects the extraction rate of stilbene substances; the reason for the reduced extraction rate in Example 6 may be that the stirring temperature is too low, which causes foam to be generated in extractant a, affecting the extraction effect of extractant a; the reason for the reduced extraction rate in Example 7 may be that the stirring speed is too fast, which also causes more foam to be generated in extractant a, thereby affecting the extraction effect of extractant a; the reason why the extraction rate in Example 8 is lower than that in Example 1 may be that the temperature is too low when the Dendrobium officinale powder is degreased, the degreasing effect is not good, and the residual fat affects the extraction of extractant a. Effect: The reason why the extraction rate in Example 9 is lower than that in Example 1 may be that the dosage of extractant a is too small, and the stilbene substances cannot be fully extracted; the reason why the extraction rate in Example 10 is lower than that in Example 1 may be that the tank group tank assembly dynamic countercurrent method is not used for extraction, resulting in a low extraction rate; the reason why the extraction rate in Example 11 is lower than that in Example 1 may be that the pH value of the aqueous phase is too high when the sodium hydroxide solution is used for treatment, and some ethylene glycol phenyl ether will be dissolved in the aqueous phase, so that some stilbene substances will be dissolved in the ethylene glycol phenyl ether organic phase during the subsequent dilute hydrochloric acid treatment, resulting in a low extraction rate of stilbene substances; the reason why the extraction rate in Example 12 is lower than that in Example 1 may be that the pH value of the aqueous phase is too high when the dilute hydrochloric acid is used for treatment, and some stilbene substances are not precipitated, resulting in a low extraction rate of stilbene substances; the reason why the extraction rate in Example 13 is lower than that in Example 1 may be that the standing time is too short, and some stilbene substances are precipitated, resulting in a low extraction rate of stilbene substances.

[0040] The solid a obtained in Example 1 was used in Examples 14 to 26 to continue extracting Dendrobium officinale polysaccharides. Embodiment 14

[0041] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.1, and deionized water was added until the water content of the system was 31%, and then the system was heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0042] The solid a is immersed in anhydrous ethanol, fully stirred, filtered and dried, and then the solid a and the extractant b are mixed at a solid-liquid ratio of 1:25 g / ml, stirred at 75°C at a speed of 250 r / min for 60 min, the filtered residue and filtrate are added with 2.5 times the volume of anhydrous ethanol after the filtrate is cooled, and alcohol precipitation is carried out at 3°C ​​for 9 hours, centrifuged at a speed of 4000 r / min for 15 minutes, and dried to obtain Dendrobium officinale polysaccharide. Embodiment 15

[0043] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.0, and deionized water was added until the water content of the system was 32%. The system was then heated to 76°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0044] The solid a was immersed in anhydrous ethanol, and after being fully stirred, it was filtered and dried. Subsequently, the solid a and the extractant b were mixed at a solid-liquid ratio of 1:26 g / ml, and stirred at 70°C at a speed of 300 r / min for 55 min. The filtered residue and filtrate were added with 2 times the volume of anhydrous ethanol after the filtrate was cooled, and the mixture was precipitated at 2°C for 8 h. The mixture was centrifuged at a speed of 3900 r / min for 16 min, and the Dendrobium officinale polysaccharide was obtained after drying. Example 16

[0045] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.2, and deionized water was added to the system until the water content was 30%, and then the system was heated to 80°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0046] The solid a is immersed in anhydrous ethanol, fully stirred, filtered and dried, and then the solid a and the extractant b are mixed at a solid-liquid ratio of 1:24 g / ml, stirred at 80°C at a speed of 200 r / min for 65 min, and the filtered residue and filtrate are added with 3 times the volume of anhydrous ethanol after the filtrate is cooled, and the mixture is precipitated at 4°C for 10 h, centrifuged at a speed of 4100 r / min for 14 min, and dried to obtain Dendrobium officinale polysaccharide. Embodiment 17

[0047] Glycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.1, and deionized water was added until the water content of the system was 31%, and then the system was heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0048] The rest is the same as Example 14. Embodiment 18

[0049] N,N-dimethylglycine and dodecyl dimethyl betaine were mixed in a molar ratio of 1:3.1, and deionized water was added until the water content of the system was 31%. The system was then heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0050] The rest is the same as Example 14. Embodiment 19

[0051] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:2, and deionized water was added until the water content of the system was 31%, and then the system was heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0052] The rest is the same as Example 14. Embodiment 20

[0053] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.1, and deionized water was added to the system until the water content was 20%, and then the system was heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0054] The rest is the same as Example 14. Embodiment 21

[0055] Solid a and extractant b were mixed at a solid-liquid ratio of 1:25 g / ml, stirred at 75°C at a speed of 250 r / min for 60 min, filtered residues and filtrate, and after the filtrate was cooled, 2.5 times the volume of anhydrous ethanol was added to the filtrate, precipitated at 3°C ​​for 9 h, centrifuged at a speed of 4000 r / min for 15 min, and dried to obtain Dendrobium officinale polysaccharide.

[0056] The rest is the same as Example 14. Embodiment 22

[0057] The solid a is immersed in anhydrous ethanol, fully stirred, filtered and dried, and then the solid a and the extractant b are mixed at a solid-liquid ratio of 1:15 g / ml, stirred at 75°C at a speed of 250 r / min for 60 min, the filtered residue and filtrate are added with 2.5 times the volume of anhydrous ethanol after the filtrate is cooled, and alcohol precipitation is carried out at 3°C ​​for 9 hours, centrifuged at a speed of 4000 r / min for 15 minutes, and dried to obtain Dendrobium officinale polysaccharide.

[0058] The rest is the same as Example 14. Embodiment 23

[0059] The solid a is immersed in anhydrous ethanol, fully stirred, filtered and dried, and then the solid a and the extractant b are mixed at a solid-liquid ratio of 1:25 g / ml, stirred at 55° C. and 250 r / min for 60 min, and the filtered residue and filtrate are added with 2.5 times the volume of anhydrous ethanol after the filtrate is cooled, and the mixture is precipitated at 3° C. for 9 h, centrifuged at 4000 r / min for 15 min, and dried to obtain Dendrobium officinale polysaccharide.

[0060] The rest is the same as Example 14. Embodiment 24

[0061] The solid a is immersed in anhydrous ethanol, fully stirred, filtered and dried, and then the solid a and the extractant b are mixed at a solid-liquid ratio of 1:25 g / ml, stirred at 65°C at a speed of 250 r / min for 60 min, and the filtered residue and filtrate are added with 1.5 times the volume of anhydrous ethanol after the filtrate is cooled, and alcohol precipitation is carried out at 3°C ​​for 9 h, and centrifuged at a speed of 4000 r / min for 15 min. After drying, Dendrobium officinale polysaccharide is obtained.

[0062] The rest is the same as Example 14. Embodiment 25

[0063] The solid a is immersed in anhydrous ethanol, fully stirred, filtered and dried, and then the solid a and the extractant b are mixed at a solid-liquid ratio of 1:25 g / ml, stirred at 65°C at a speed of 250 r / min for 60 min, and the filtered residue and filtrate are added with 70% volume fraction ethanol solution in an amount of 2.5 times the volume of the filtrate after the filtrate is cooled, and alcohol precipitation is carried out at 10°C for 9 h, and centrifuged at a speed of 4000 r / min for 15 min. After drying, Dendrobium officinale polysaccharide is obtained.

[0064] The rest is the same as Example 14.

[0065] Test 2: The mass M1 of the solid a and the mass m1 of the obtained Dendrobium officinale polysaccharide in Examples 14 to 25 were measured, and the extraction rate of the Dendrobium officinale polysaccharide in each example was calculated by the formula b=m1 / M1. The specific data are shown in Table 2.

[0066] Table 2 Extraction rate of polysaccharides from Dendrobium officinale in Examples 14 to 25 Implementation items Extraction rate of polysaccharides from Dendrobium officinale b (%) Embodiment 14 33.42 Embodiment 15 33.38 Example 16 33.35 Embodiment 17 26.44 Embodiment 18 27.19 Embodiment 19 30.52 Embodiment 20 30.06 Embodiment 21 31.92 Embodiment 22 29.44 Embodiment 23 30.93 Embodiment 24 28.20 Embodiment 25 32.11 It can be seen from Table 2 that the extraction rate of Dendrobium officinale polysaccharide in Examples 14 to 16 is the highest; the reason why the extraction rate in Example 17 is significantly reduced may be that after the low eutectic solvent component is replaced with glycine, due to the poor thermal stability of glycine, a part of it will be lost during the preparation process and a part of it will be lost during the extraction process, which affects the properties of the low eutectic solvent and reduces its extraction effect; the reason why the extraction rate in Example 18 is significantly reduced may be that after the low eutectic solvent component is replaced with dodecyl dimethyl betaine, because it also has excellent thickening properties, it will further increase the viscosity of the low eutectic solvent, reduce its dissolving ability, and thus affect the extraction effect; the reason why the extraction rate in Example 19 is lower than that in Example 14 may be that the molar ratio of N,N-dimethylglycine to tetradecyl hydroxypropyl phosphate betaine in the low eutectic solvent is relatively small, its viscosity and surface tension are relatively large, and its dissolving ability is reduced; the extraction rate in Example 20 The reason for the lower extraction rate than that of Example 14 may be that the water content of the low eutectic solvent system is relatively low, the viscosity is relatively large, and the solubility is reduced; the reason for the lower extraction rate of Example 21 than that of Example 14 may be that the solid a is not washed, and the residual ethylene glycol phenyl ether has an impact on the low eutectic solvent; the reason for the lower extraction rate of Example 22 than that of Example 14 may be that the solid-liquid ratio is relatively small, the dosage of the extractant b is insufficient, and the Dendrobium officinale polysaccharide cannot be fully extracted; the reason for the lower extraction rate of Example 23 than that of Example 14 may be that the extraction temperature is relatively low, which makes the viscosity of the low eutectic solvent relatively large and reduces its solubility; the reason for the lower extraction rate of Example 24 than that of Example 14 may be that the amount of anhydrous ethanol used is relatively small, resulting in a low ethanol concentration after addition, and the precipitation effect of polysaccharides is not good; the reason for the lower extraction rate of Example 25 than that of Example 14 may be that the alcohol precipitation temperature is relatively high, which prolongs the alcohol precipitation time, and thus some polysaccharides are not precipitated. Embodiment 26

[0067] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.1, and deionized water was added until the water content of the system was 31%, and then the system was heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0068] 0.4 parts of octyl glucoside were added to 9.5 parts of ethylene glycol phenyl ether, followed by stirring at 45°C and 150 r / min for 11 minutes, and then cooling to obtain extractant a.

[0069] 2.5 parts of chicoric acid and 1.5 parts of salvianolic acid B were added to 35 parts of deionized water, and stirred evenly at 25° C. to obtain a water-soluble stabilizer.

[0070] The nutrient solution is obtained by uniformly mixing water, urea and glucose in a mass ratio of 1:0.03:0.03.

[0071] (1) Weigh the powder of Dendrobium officinale, add 9 times the weight of petroleum ether to degrease at 45°C, add 6 times the weight of extractant a with wetting and dual surfactant properties to the powder, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.02, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.2. After sufficient stirring, let it stand for 2.5 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain Dendrobium officinale stilbene-like substances.

[0072] (2) Immerse solid a in anhydrous ethanol, stir thoroughly, filter and dry, then mix solid a and extractant b at a solid-liquid ratio of 1:25 g / ml, stir at 75°C and 250 r / min for 60 min, filter the residue and filtrate, add 2.5 times the volume of anhydrous ethanol to the filtrate after the filtrate is cooled, perform alcohol precipitation at 3°C ​​for 9 h, centrifuge at 4000 r / min for 15 min, and obtain Dendrobium officinale polysaccharide after drying.

[0073] (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.11, and then a nutrient solution of 2.5 times the mass of the filter residue is added, and fermented at 34°C for 5.5 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 9 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substances and the Dendrobium officinale polysaccharides obtained in step (1) and step (2) are added to the fermentation liquid, and the mixture is stirred evenly. Then, a water-soluble stabilizer of 6% by mass of the liquor is added, and the mixture is stirred until uniform, and then sterilized and canned to obtain the Dendrobium officinale medicinal liquor. Embodiment 27

[0074] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.1, and deionized water was added until the water content of the system was 31%, and then the system was heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0075] 0.4 parts of octyl glucoside were added to 9.5 parts of ethylene glycol phenyl ether, followed by stirring at 45°C and 150 r / min for 11 minutes, and then cooling to obtain extractant a.

[0076] Add 2 parts of chicoric acid and 2 parts of salvianolic acid B into 30 parts of deionized water, and stir evenly at 20° C. to obtain a water-soluble stabilizer.

[0077] The nutrient solution was obtained by uniformly mixing water, urea and glucose in a mass ratio of 1: 0.04:0.02.

[0078] (1) Weigh the powder of Dendrobium officinale, add 9 times the weight of petroleum ether to degrease at 45°C, add 6 times the weight of extractant a with wetting and dual surfactant properties to the powder, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.02, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.2. After sufficient stirring, let it stand for 2.5 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain Dendrobium officinale stilbene-like substances.

[0079] (2) Immerse solid a in anhydrous ethanol, stir thoroughly, filter and dry, then mix solid a and extractant b at a solid-liquid ratio of 1:25 g / ml, stir at 75°C and 250 r / min for 60 min, filter the residue and filtrate, add 2.5 times the volume of anhydrous ethanol to the filtrate after the filtrate is cooled, perform alcohol precipitation at 3°C ​​for 9 h, centrifuge at 4000 r / min for 15 min, and obtain Dendrobium officinale polysaccharide after drying.

[0080] (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.1, and then a nutrient solution of 3 times the mass of the filter residue is added, and fermented at 33° C. for 6 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 8 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substances and the Dendrobium officinale polysaccharides obtained in step (1) and step (2) are added to the fermentation liquid, and the mixture is stirred evenly. A water-soluble stabilizer of 7% by mass of the liquor is then added, and the mixture is stirred until uniformly mixed, and then sterilized and canned to obtain the Dendrobium officinale medicinal liquor. Embodiment 28

[0081] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.1, and deionized water was added until the water content of the system was 31%, and then the system was heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0082] 0.4 parts of octyl glucoside were added to 9.5 parts of ethylene glycol phenyl ether, followed by stirring at 45°C and 150 r / min for 11 minutes, and then cooling to obtain extractant a.

[0083] Add 3 parts of chicoric acid and 1 part of salvianolic acid B into 40 parts of deionized water, and stir evenly at 30° C. to obtain a water-soluble stabilizer.

[0084] The nutrient solution is obtained by uniformly mixing water, urea and glucose in a mass ratio of 1:0.02:0.04.

[0085] (1) Weigh the powder of Dendrobium officinale, add 9 times the weight of petroleum ether to degrease at 45°C, add 6 times the weight of extractant a with wetting and dual surfactant properties to the powder, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.02, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.2. After sufficient stirring, let it stand for 2.5 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain Dendrobium officinale stilbene-like substances.

[0086] (2) Immerse solid a in anhydrous ethanol, stir thoroughly, filter and dry, then mix solid a and extractant b at a solid-liquid ratio of 1:25 g / ml, stir at 75°C and 250 r / min for 60 min, filter the residue and filtrate, add 2.5 times the volume of anhydrous ethanol to the filtrate after the filtrate is cooled, perform alcohol precipitation at 3°C ​​for 9 h, centrifuge at 4000 r / min for 15 min, and obtain Dendrobium officinale polysaccharide after drying.

[0087] (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.12, and then a nutrient solution of 2 times the mass of the filter residue is added, and fermented at 35° C. for 5 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 10 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substances and the Dendrobium officinale polysaccharides obtained in step (1) and step (2) are added to the fermentation liquid, and the mixture is stirred evenly. A water-soluble stabilizer of 5% by mass of the liquor is then added, and the mixture is stirred until uniform, and then sterilized and canned to obtain the Dendrobium officinale medicinal liquor. Embodiment 29

[0088] Add 4 parts of chicoric acid to 35 parts of deionized water and stir evenly at 25°C to obtain a water-soluble stabilizer.

[0089] The rest is the same as Example 26. Embodiment 30

[0090] 4 parts of salvianolic acid B were added into 35 parts of deionized water and stirred evenly at 25° C. to obtain a water-soluble stabilizer.

[0091] The rest is the same as Example 26. Embodiment 31

[0092] Add 2.5 parts of ferulic acid and 1.5 parts of salvianolic acid B into 35 parts of deionized water, and stir evenly at 25° C. to obtain a water-soluble stabilizer.

[0093] The rest is the same as Example 26. Embodiment 32

[0094] 2.5 parts of chicoric acid and 1.5 parts of caffeic acid were added to 35 parts of deionized water, and stirred evenly at 25° C. to obtain a water-soluble stabilizer. Embodiment 33

[0095] 2.5 parts of chicoric acid and 1.5 parts of salvianolic acid B were added into 50 parts of deionized water, and stirred evenly at 25° C. to obtain a water-soluble stabilizer.

[0096] The rest is the same as Example 26. Embodiment 34

[0097] (1) Weigh the powder of Dendrobium officinale, add 9 times the weight of petroleum ether to degrease at 45°C, add 6 times the weight of extractant a with wetting and dual surfactant properties to the powder, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.02, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.2. After sufficient stirring, let it stand for 2.5 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain Dendrobium officinale stilbene-like substances.

[0098] (2) Immerse solid a in anhydrous ethanol, stir thoroughly, filter and dry, then mix solid a and extractant b at a solid-liquid ratio of 1:25 g / ml, stir at 75°C and 250 r / min for 60 min, filter the residue and filtrate, add 2.5 times the volume of anhydrous ethanol to the filtrate after the filtrate is cooled, perform alcohol precipitation at 3°C ​​for 9 h, centrifuge at 4000 r / min for 15 min, and obtain Dendrobium officinale polysaccharide after drying.

[0099] (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.3, and then a nutrient solution of 2.5 times the mass of the filter residue is added, and fermented at 34°C for 5.5 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 9 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substances and the Dendrobium officinale polysaccharides obtained in step (1) and step (2) are added to the fermentation liquid, and the mixture is stirred evenly. Then, a water-soluble stabilizer of 6% by mass of the liquor is added, and the mixture is stirred until uniform, and then sterilized and canned to obtain the Dendrobium officinale medicinal liquor.

[0100] The rest is the same as Example 26. Embodiment 35

[0101] (1) Weigh the powder of Dendrobium officinale, add 9 times the weight of petroleum ether to degrease at 45°C, add 6 times the weight of extractant a with wetting and dual surfactant properties to the powder, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.02, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.2. After sufficient stirring, let it stand for 2.5 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain Dendrobium officinale stilbene-like substances.

[0102] (2) Immerse solid a in anhydrous ethanol, stir thoroughly, filter and dry, then mix solid a and extractant b at a solid-liquid ratio of 1:25 g / ml, stir at 75°C and 250 r / min for 60 min, filter the residue and filtrate, add 2.5 times the volume of anhydrous ethanol to the filtrate after the filtrate is cooled, perform alcohol precipitation at 3°C ​​for 9 h, centrifuge at 4000 r / min for 15 min, and obtain Dendrobium officinale polysaccharide after drying.

[0103] (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.11, and then a nutrient solution of 2.5 times the mass of the filter residue is added, and fermented at 45°C for 5.5 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 9 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substances and the Dendrobium officinale polysaccharides obtained in step (1) and step (2) are added to the fermentation liquid, and the mixture is stirred evenly. Then, a water-soluble stabilizer of 6% by mass of the liquor is added, and the mixture is stirred until uniform, and then sterilized and canned to obtain the Dendrobium officinale medicinal liquor.

[0104] The rest is the same as Example 26. Embodiment 36

[0105] (1) Weigh the powder of Dendrobium officinale, add 9 times the weight of petroleum ether to degrease at 45°C, add 6 times the weight of extractant a with wetting and dual surfactant properties to the powder, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.02, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.2. After sufficient stirring, let it stand for 2.5 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain Dendrobium officinale stilbene-like substances.

[0106] (2) Immerse solid a in anhydrous ethanol, stir thoroughly, filter and dry, then mix solid a and extractant b at a solid-liquid ratio of 1:25 g / ml, stir at 75°C and 250 r / min for 60 min, filter the residue and filtrate, add 2.5 times the volume of anhydrous ethanol to the filtrate after the filtrate is cooled, perform alcohol precipitation at 3°C ​​for 9 h, centrifuge at 4000 r / min for 15 min, and obtain Dendrobium officinale polysaccharide after drying.

[0107] (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.11, and then a nutrient solution of 2.5 times the mass of the filter residue is added, and fermented at 34°C for 8 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 9 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substances and the Dendrobium officinale polysaccharides obtained in step (1) and step (2) are added to the fermentation liquid, and the mixture is stirred evenly. Then, a water-soluble stabilizer of 6% by mass of the liquor is added, and the mixture is stirred until uniform, and then sterilized and canned to obtain the Dendrobium officinale medicinal liquor.

[0108] The rest is the same as Example 26. Embodiment 37

[0109] (1) Weigh the powder of Dendrobium officinale, add 9 times the weight of petroleum ether to degrease at 45°C, add 6 times the weight of extractant a with wetting and dual surfactant properties to the powder, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.02, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.2. After sufficient stirring, let it stand for 2.5 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain Dendrobium officinale stilbene-like substances.

[0110] (2) Immerse solid a in anhydrous ethanol, stir thoroughly, filter and dry, then mix solid a and extractant b at a solid-liquid ratio of 1:25 g / ml, stir at 75°C and 250 r / min for 60 min, filter the residue and filtrate, add 2.5 times the volume of anhydrous ethanol to the filtrate after the filtrate is cooled, perform alcohol precipitation at 3°C ​​for 9 h, centrifuge at 4000 r / min for 15 min, and obtain Dendrobium officinale polysaccharide after drying.

[0111] (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.11, and then a nutrient solution of 2.5 times the mass of the filter residue is added, and fermented at 34°C for 5.5 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 9 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substances and the Dendrobium officinale polysaccharides obtained in step (1) and step (2) are added to the fermentation liquid, and the mixture is stirred evenly. A water-soluble stabilizer of 2% by mass of the liquor is then added, and the mixture is stirred until uniform, and then sterilized and canned to obtain the Dendrobium officinale medicinal liquor.

[0112] The rest is the same as Example 26. Embodiment 38

[0113] N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.1, and deionized water was added until the water content of the system was 31%, and then the system was heated to 78°C and stirred continuously until a uniform and transparent solution was obtained. After cooling, extract b was obtained.

[0114] 0.4 parts of octyl glucoside were added to 9.5 parts of ethylene glycol phenyl ether, followed by stirring at 45°C and 150 r / min for 11 minutes, and then cooling to obtain extractant a.

[0115] The nutrient solution is obtained by uniformly mixing water, urea and glucose in a mass ratio of 1:0.03:0.03.

[0116] (1) Weigh the powder of Dendrobium officinale, add 9 times the weight of petroleum ether to degrease at 45°C, add 6 times the weight of extractant a with wetting and dual surfactant properties to the powder, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.02, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.2. After sufficient stirring, let it stand for 2.5 hours, centrifuge to obtain the precipitate, and wash with deionized water to obtain Dendrobium officinale stilbene-like substances.

[0117] (2) Immerse solid a in anhydrous ethanol, stir thoroughly, filter and dry, then mix solid a and extractant b at a solid-liquid ratio of 1:25 g / ml, stir at 75°C and 250 r / min for 60 min, filter the residue and filtrate, add 2.5 times the volume of anhydrous ethanol to the filtrate after the filtrate is cooled, perform alcohol precipitation at 3°C ​​for 9 h, centrifuge at 4000 r / min for 15 min, and obtain Dendrobium officinale polysaccharide after drying.

[0118] (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.11, and then a nutrient solution of 2.5 times the mass of the filter residue is added, and fermented at 34°C for 5.5 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 9 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substance obtained in step (1) and step (2) and the Dendrobium officinale polysaccharide are added to the fermentation liquid, and the mixture is uniformly stirred and sterilized and canned to obtain the Dendrobium officinale medicinal wine.

[0119] Test 3: The Dendrobium Officinale Wine prepared in Examples 26 to 38 was placed at 50°C for 4 hours on the first day, naturally cooled to room temperature, and then placed under an illumination of 3000Lx for 2 hours. After the treatment, the Dendrobium Officinale Wine was placed in a 0°C environment for 4 hours. When the temperature rose to room temperature, the Dendrobium Officinale Wine was stirred at a speed of 200r / min for 15 minutes, and then allowed to stand for 4 hours to observe whether the Dendrobium Officinale Wine showed color changes and precipitation. The Dendrobium Officinale Wine was treated continuously for 10 days according to this treatment method, and the time when the color change and precipitation of the wine were recorded. After 10 days, the transmittance of the wine without precipitation was measured. The specific data are shown in Table 3.

[0120] Table 3 Stability data of Dendrobium officinale medicinal wine of Examples 26 to 38 Implementation items Transmittance before treatment (%) Transmittance after treatment (%) Time of changes in medicinal wine phenomena Embodiment 26 87.6 86.2 The light yellow wine has no color change and no precipitation Embodiment 27 87.3 86.0 The light yellow wine has no color change and no precipitation Embodiment 28 87.4 85.8 The light yellow wine has no color change and no precipitation Embodiment 29 87.1 / On the third day, it turns from light yellow to yellow and precipitates on the third day. Embodiment 30 86.9 / On the third day, it turns from light yellow to yellow and precipitates on the third day. Embodiment 31 82.6 / On the fourth day, it changes from light yellow to yellow and precipitates on the fourth day. Embodiment 32 81.8 / On the fourth day, it changes from light yellow to yellow and precipitates on the fourth day. Embodiment 33 87.3 83.8 The light yellow wine has no color change and no precipitation Embodiment 34 81.2 / On the seventh day, it turns from light yellow to yellow, and on the eighth day, precipitation occurs. Embodiment 35 82.5 / On the eighth day, it turns from light yellow to yellow, and on the ninth day, precipitation occurs. Embodiment 36 80.8 / On the seventh day, it turns from light yellow to yellow, and on the eighth day, precipitation occurs. Embodiment 37 87.2 81.5 On the ninth day, it changes from light yellow to yellow with no precipitation Embodiment 38 87.0 / The next day, it turns from light yellow to yellow and a precipitate forms on the next day. It can be seen from Table 3 that the transmittance of the Dendrobium Officinale Wine obtained in Examples 26 to 28 changes the least and no obvious phenomenon occurs; Examples 29 and 30 respectively use only one component as a stabilizer, but their stability effects are only slightly better than that of Example 38 which does not use a stabilizer, indicating that a single antioxidant is not effective in enhancing the stability of the wine; Examples 31 and 32 replace the stabilizer component, and the water solubility of the replaced component is poor and cannot be completely integrated with the wine, which affects the transmittance of the wine on the one hand, and on the other hand cannot effectively exert its antioxidant and acidity, and cannot effectively enhance the stability of the Dendrobium Officinale Wine; The reason why the stability of the Dendrobium Officinale Wine in Example 33 is not as good as that in Example 26 may be that the amount of deionized water added is too large, which reduces the concentration of the active ingredient in the stabilizer; The reason why the stability of Dendrobium Officinale Wine is not as good as that of Example 26 may be that the amount of yeast added is too much, resulting in excessive fermentation, which will produce more impurities and affect the stability of the wine; the reason why the stability of Dendrobium Officinale Wine is not as good as that of Example 26 may be that the fermentation temperature is too high, the fermentation effect is not good, and the carbon source and nitrogen source in the nutrient solution will affect the stability of the wine; the reason why the stability of Dendrobium Officinale Wine is not as good as that of Example 26 may be that the fermentation time is too long, resulting in excessive fermentation, which will produce more impurities and affect the stability of the wine; the reason why the stability of Dendrobium Officinale Wine is not as good as that of Example 26 may be that the amount of water-soluble stabilizer added is too small, and the stabilization effect is weak; Example 38 does not add water-soluble stabilizer, so its stability performance is the worst among Examples 26 to 38.

Claims

1. A medicinal wine containing Dendrobium officinale, characterized in that: The specific preparation method is: (1) Weigh the powder of Dendrobium officinale, add 8 to 10 times the weight of petroleum ether to degrease at 40 to 50°C, add the powder of Dendrobium officinale to 5 to 7 times the weight of extractant a having wetting and dual surfactant properties, and then extract it by tank-type tank assembly dynamic countercurrent method. After the extraction, solid a and extract are separated, dilute sodium hydroxide solution is added to the extract and stirred until the pH value of the aqueous phase is 7.01 to 7.03, the organic phase is separated and recycled, and dilute hydrochloric acid is added to the aqueous phase until the pH value is 5.0 to 5.

4. After sufficient stirring, let it stand for 2 to 3 hours, centrifuge to obtain the precipitate, and wash it with deionized water to obtain the Dendrobium officinale stilbene-like substance; (2) solid a is immersed in anhydrous ethanol, fully stirred, filtered and dried, then solid a and low-viscosity and highly stable extractant b are mixed at a solid-liquid ratio of 1:24-26 g / ml, stirred at 70-80°C at a speed of 200-300 r / min for 55-65 min, filtered residue and filtrate, after the filtrate is cooled, 2-3 times the volume of anhydrous ethanol is added to the filtrate, precipitated at 2-4°C for 8-10 h, centrifuged at a speed of 3900-4100 r / min for 14-16 min, and dried to obtain Dendrobium officinale polysaccharide; (3) The filter residue and yeast are uniformly mixed in a mass ratio of 1:0.1-0.12, and then a nutrient solution of 2-3 times the mass of the filter residue is added, and fermented at 33-35° C. for 5-6 days. After the fermentation is completed, the fermentation liquid is filtered to obtain a fermentation liquid, and then 8-10 times the volume of 50-proof edible liquor, the Dendrobium officinale stilbene substance obtained in step (1) and step (2) and the Dendrobium officinale polysaccharide are added to the fermentation liquid, and the mixture is uniformly stirred, sterilized and canned to obtain the Dendrobium officinale medicinal wine.

2. The medicinal wine containing Dendrobium officinale as claimed in claim 1, characterized in that: The preparation method of the extractant a is: 0.3-0.5 parts of octyl decyl glucoside are added to 9-10 parts of ethylene glycol phenyl ether, followed by stirring at 40-50°C at a speed of 100-200 r / min for 10-12 minutes, and then cooling to obtain extractant a.

3. The medicinal wine containing Dendrobium officinale as claimed in claim 1, characterized in that: The tank group tank assembly dynamic countercurrent method is specifically: In the first extraction of the first tank of Dendrobium officinale powder, 5 to 7 times the mass of the extractant a is added, and in the second and third extractions, 5 to 7 times and 2 to 4 times the mass of the extractant a are added respectively; after the first tank extraction is completed, new Dendrobium officinale powder is added to the second tank, and the extract obtained from the second extraction in the first tank is added as the extractant to the second tank for the first extraction, and in the second extraction in the second tank, the extract obtained from the third extraction in the first tank is used as the extractant and the extractant a is supplemented to the same volume as the first extraction in the second tank, and 2 to 4 times the mass of the extractant a is added to the third extraction of Dendrobium officinale powder; the extraction method of the third tank is the same as that of the second tank, and the second extraction and the third extraction in the second tank are used as the first and second extractions in the third tank, respectively, and 3 to 5 times the mass of the extractant a is added to the third extraction of Dendrobium officinale powder; Among them, each extraction time is 60~80min, the extraction temperature is 65~70℃, and the stirring speed is 80~100r / min.

4. The medicinal wine containing Dendrobium officinale as claimed in claim 1, characterized in that: The preparation method of the extractant b is: N,N-dimethylglycine and tetradecyl hydroxypropyl betaine phosphate were mixed in a molar ratio of 1:3.0-3.2, and deionized water was added until the water content of the system was 30%-32%, and then the system was heated to 76-80°C and stirred continuously until a uniform and transparent solution was obtained, and then the extract b was obtained after cooling.

5. The medicinal wine containing Dendrobium officinale as claimed in claim 1, characterized in that: The nutrient solution is: The product is obtained by uniformly mixing water, urea and glucose in a mass ratio of 1:0.02~0.04:0.02~0.

04.

6. A water-soluble stabilizer for the medicinal wine containing Dendrobium officinale as claimed in claim 1, characterized in that: The specific preparation steps are: Add 2-3 parts of chicoric acid and 1-2 parts of salvianolic acid B into 30-40 parts of deionized water, and stir evenly at 20-30°C to obtain a water-soluble stabilizer.

7. A water-soluble stabilizer as claimed in claim 6, characterized in that: The mass ratio of Dendrobium officinale medicinal wine and water-soluble stabilizer is 1:0.05~0.07.