Preparation process of cordyceps militaris powder

Abstract

The application discloses a preparation process of Cordyceps militaris powder. The Cordyceps militaris is extracted by using an ultrasonic coupling enzymatic extraction method, so that the obtained Cordyceps militaris polysaccharide component has high content and good antioxidant activity. In the process of adsorbing and purifying the Cordyceps militaris extraction liquid by using cellulose microspheres, the cellulose microspheres are subjected to a graft modification treatment, so that additional adsorption sites are increased, adsorption of organic impurities is increased, and adsorption of the polysaccharide component is reduced. In the subsequent powder preparation process, a wetting regulator is used to improve the wetness of the powder and the hygroscopicity caused by the cellulose molecules, so that the uniformity, fineness and flowability of the Cordyceps militaris powder quality are ensured.

Description

Technical Field

[0001] This invention relates to the field of powder preparation, and in particular to a preparation process for Cordyceps militaris powder. Background Technology

[0002] Cordyceps militaris, also known as North Cordyceps sinensis, is a fungus belonging to the order Clavicipitales, family Clavicipitaceae, and genus Cordyceps. It contains various effective components such as cordycepin, polysaccharides, and cordycepic acid, and has good effects in regulating immunity, anti-inflammation, antiviral, anti-cancer, and anti-aging.

[0003] Currently, the traditional method for polysaccharide extraction is hot water extraction, but this method has drawbacks such as high extraction temperature, long extraction time, and low extraction rate. Furthermore, it consumes a large amount of extraction solvent, requiring repeated vacuum concentration of the large volume of extract obtained after multiple extractions, which increases the complexity of subsequent processes. Therefore, more and more novel extraction technologies are being applied to extraction processes.

[0004] Crude polysaccharide extracts often contain various impurities, such as pigments, proteins, oligosaccharides, pectin, polyphenols, and flavonoids. Due to their low purity, they fail to meet the requirements for practical applications, significantly impacting the accuracy of polysaccharide structure analysis and bioactivity studies. Therefore, removing impurities to obtain high-purity polysaccharides with good homogeneity is crucial. Traditional purification methods for Cordyceps militaris polysaccharides include crystallization and solvent extraction. In recent years, chromatographic separation, ion exchange resins, and macroporous adsorption resins have become commonly used for separation and purification.

[0005] Cellulose microspheres are insoluble in water and common organic solvents, exhibiting good chemical stability. Due to the large number of hydroxyl groups in cellulose microspheres, they possess excellent hydrophilicity and biocompatibility, providing a milder environment compared to other hydrophobic materials (such as silicon). Cellulose is the world's most abundant renewable resource, inexpensive, and possesses advantages such as non-toxicity, biodegradability, and good biocompatibility. However, natural cellulose substrates cannot meet the performance requirements of specific materials, often requiring surface modification to broaden their applicability.

[0006] The powder formulation consists of raw materials, various adjuvants, and other substances mixed in a specific ratio, and then pulverized into fine powder using a specific machine according to particle size requirements. Due to the complexity of Cordyceps militaris components, there are significant differences in particle size distribution, flowability, and viscosity among different preparation processes during powder preparation. Developing a suitable powder preparation process is the focus of this invention. Summary of the Invention

[0007] To solve the above-mentioned technical problems, the present invention provides a preparation process for Cordyceps militaris.

[0008] The specific preparation process is as follows:

[0009] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 20-25 parts of Cordyceps militaris powder and add 400-500 parts of a mixed solution of cellulase, complexing agent and water in a certain mass ratio. Perform enzymatic hydrolysis for 1-2 hours. Then, use a water bath at 50℃ and ultrasonic power of 500w for 40-50 minutes. Then, centrifuge and filter at 3000r / min to obtain Cordyceps militaris extract.

[0010] The complexing agent is sodium R-3-hydroxybutyrate; the mass ratio of cellulase, complexing agent and water is 1:0.1:20.

[0011] (2) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 30-50 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0012] (3) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of (-0.8)-(-0.4) MPa to obtain a concentrated extract with a water content of 20%. 10%-20% of the concentrated extract mass of dextrin and 6%-9% of fructose are added to it, and the stirring speed is 100-140 r / min.

[0013] (3) Crushing: After the above powder is stirred for 20-30 minutes, spray 3.15-7.15 parts of wetting and conditioning solution in 3-5 times. Continue stirring for 5-8 minutes and then transfer it to an air jet mill with an air flow rate of 300-500 m / min. Cordyceps militaris powder is obtained when it flows out.

[0014] The grafted and modified cellulose microspheres in step (2) are prepared as follows:

[0015] 1) Immobilization of cellulose microspheres with initiator: Take 0.6-0.8 parts of cellulose microspheres and ultrasonically wash them for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 6-8 parts of initiator, 3-5 parts of TEA, 0.16-0.2 parts of DMAP and 0.2-0.25 parts of THF. React in a constant temperature oil bath at 25℃ for 24 h with magnetic stirring at 100 r / min. After reaction, ultrasonically wash the cellulose microspheres three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then vacuum dry them at 40℃ for 24 h and store them in a desiccator.

[0016] The initiator is methyl pyruvate;

[0017] 2) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 20-25 parts anisole, 20-25 parts grafting agent, 0.09-0.15 parts methyl pyruvate, 0.01-0.02 CuBr2, and 0.08-0.12 PMDETA. After the addition is complete, bubble with N2 for 15 min, and react in a constant temperature water bath at 30℃ for 4 h. Then add 30-40 parts dichloromethane to dilute, centrifuge and filter out the cellulose microspheres, and ultrasonically wash twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol respectively. After washing, vacuum dry the grafted microspheres at 40℃ for 24 h and store them in a desiccator.

[0018] The grafting agent is 1-(4-aminobenzyl)imidazol.

[0019] The wetting conditioning solution in step (4) is prepared as follows: Prepare 2-5 parts of water and heat it to 40°C. First, add 0.3-0.8 parts of ethanol, 0.5-0.8 parts of sodium carboxymethyl starch, and 0.05 parts of povidone K30. Then, heat it to 50°C and add the wetting conditioner.

[0020] The wetting regulator is spermidine trihydrochloride; preferably, the wetting regulator is 0.3-0.5 parts.

[0021] The beneficial effects of this invention are as follows:

[0022] 1. This invention employs an ultrasonic-coupled enzymatic extraction method to extract Cordyceps militaris, resulting in a high content of Cordyceps militaris polysaccharides with excellent antioxidant activity. During the adsorption and purification of the Cordyceps militaris extract using cellulose microspheres, the microspheres undergo graft modification to increase additional adsorption sites, enhance the adsorption of organic impurities, and reduce the adsorption of polysaccharides. In the subsequent powder preparation process, a wetting regulator is used to improve the wettability of the powder and reduce the hygroscopicity caused by cellulose molecules, ensuring the uniformity, fineness, and flowability of the Cordyceps militaris powder.

[0023] 2. In the research on the extraction process of Cordyceps militaris, water was chosen as the extraction solvent instead of other solvents such as ethanol. This is mainly because, in addition to cordycepin, Cordyceps militaris also contains polysaccharides, which play a very important role in improving immunity.

[0024] 3. Enzymatic hydrolysis is a mild and highly selective method. During the extraction process, adding appropriate enzymes can break down the cell wall, allowing for more effective release of polysaccharide components from the cell wall and cells, thus increasing the extraction rate. Ultrasonic coupling with enzymatic hydrolysis enhances the extraction of Cordyceps militaris, which not only increases the polysaccharide content of Cordyceps militaris but also shortens the extraction time. The polysaccharide yield is more than twice that of hot water extraction, and the antioxidant activity is the best.

[0025] 4. The complexing agent sodium R-3-hydroxybutyrate can form complexes with substrates or products, increasing their stability and solubility in solution, thereby improving the conversion rate of the substrate. Sodium R-3-hydroxybutyrate can bind with metal ions present in Cordyceps militaris to form stable complexes, reducing the inhibitory effect of metal ions on enzymes, helping to maintain enzyme activity, improving the efficiency of enzyme catalytic reaction, and providing a certain acidic environment to adjust the pH value of the reaction system, providing the most suitable reaction conditions for cellulase activity, and optimizing the effect of enzymatic hydrolysis reaction.

[0026] 5. This invention employs the ARGET ATRP method to graft 1-(4-aminobenzyl)imidazol onto the surface of regenerated cellulose microspheres with good pore structure and large specific surface area. The polymer obtained by adding the sacrificial initiator methyl pyruvate, utilizes the excellent ionic solvent composition of anisole, MMA, methyl pyruvate, CuBr2, and PMDETA. The methyl pyruvate molecular chains can freely extend within this solvent, allowing the relatively stable active monomers within the molecule to readily participate and initiate the polymerization reaction. Furthermore, methyl pyruvate provides additional active free radicals, enabling rapid reaction with free radicals on the cellulose microsphere matrix, thus achieving grafting. Introducing active monomers into the cellulose microspheres and increasing intermolecular hydrogen bonds enhances the rigidity of the cellulose. Therefore, the cellulose microspheres prepared by this invention exhibit higher mechanical strength than gel chromatography, allowing for the coupling of various ligands with the cellulose for multifunctional chromatographic separation.

[0027] 6.1-(4-aminobenzyl)imidazolium can polymerize rapidly and efficiently in a simple environment with the help of methyl pyruvate. Compared with traditional initiators, it has advantages in reaction rate and aggregation effect. The 1-(4-aminobenzyl)imidazolium molecule has a stable structure and can selectively initiate grafting reactions on some functional groups in cellulose molecules, thereby achieving precise control over the structure and properties of the material.

[0028] 7. The modified cellulose derivative microspheres possess an internal porous structure. The introduction of specific hydrophobic regulating groups from 1-(4-aminobenzyl)imidazolium allows for interaction between these hydrophobic groups and polysaccharide molecules, reducing the adsorption of polysaccharide components. Furthermore, the hydrophobic groups provide additional adsorption sites, enhancing the adsorption of organic impurities. They also exhibit excellent adsorption-resorption and reuse properties, reducing the cost of the separation and purification process. This enables the modified cellulose microspheres to more effectively adsorb and separate active ingredients from traditional Chinese medicine, improving separation efficiency and purification effectiveness. The cellulose microspheres produced in this process are green, non-toxic, and environmentally friendly.

[0029] 8. The impact of the high-speed jet stream in the airflow pulverizer results in a large contact area between the material and the blades, leading to a good pulverizing effect and producing fine, uniform powder particles with high flowability.

[0030] 9. Spermine trihydrochloride exhibits high stability under high temperature and common humidity conditions. Compared to similar regulators, it is less prone to decomposition or loss of activity, and it possesses strong buffering properties, enhancing the stability of the active ingredients in Cordyceps militaris. Through a spraying process during stirring, the droplets initially wet the powder upon contact, causing it to aggregate and form particle nuclei. Spermine trihydrochloride can absorb and store moisture from the surrounding environment to a certain extent, releasing moisture when humidity is high and absorbing moisture when humidity is low, thereby maintaining the humidity balance of the extract material and ensuring the stability of the powder product.

[0031] 10. Because the extract of Cordyceps militaris contains a large number of small cellulose molecules after enzymatic hydrolysis, these smaller cellulose molecules are not easily adsorbed and removed during the adsorption and separation process. They are prone to absorbing moisture, softening, clumping, and adhering during the preparation of powder. This results in the mixture requiring more power and time to pulverize. By adding a small amount of spermidine trihydrochloride to the wetting conditioning solution, the fine particles are more evenly dispersed throughout the formulation through interaction with other components. This improves the clumping and adhesion between particles, ensuring the quality of the powder product. Furthermore, with the synergy of other excipients, the particle size distribution and powder flowability are greatly improved. Detailed Implementation

[0032] The present invention will be further described in detail below with reference to the embodiments.

[0033] Unless otherwise specified, the raw materials or chemical reagents used in the embodiments of this invention are obtained through conventional commercial channels.

[0034] Example 1

[0035] The model of the air jet mill is QL10. The specific steps are as follows:

[0036] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 22 parts of Cordyceps militaris powder and add 450 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 1.5 h, then water bath at 50 ℃, ultrasonic power of 500 W, treatment time of 45 min, and then centrifuge and filter at 3000 r / min to obtain Cordyceps militaris extract;

[0037] (2) Immobilization of cellulose microspheres as initiators: Take 0.7 parts of cellulose microspheres and wash them ultrasonically for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 7 parts of methyl pyruvate, 4 parts of TEA, 0.18 parts of DMAP and 0.22 parts of THF. React in a constant temperature oil bath at 25℃ for 24 h with magnetic stirring at 100 r / min. After the reaction, wash the cellulose microspheres ultrasonically three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then, vacuum dry them at 40℃ for 24 h and store them in a desiccator.

[0038] (3) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 22 parts of anisole, 22 parts of 1-(4-aminobenzyl)imidazol, 0.12 parts of methyl pyruvate, 0.015 CuBr2, and 0.1 PMDETA. After the addition is completed, bubbling with N2 for 15 min, constant temperature water bath at 30℃, react for 4 h, add 35 parts of dichloromethane to dilute, centrifuge and filter out the cellulose microspheres, and ultrasonically wash twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol respectively. After washing, the grafted microspheres are vacuum dried at 40℃ for 24 h and stored in a desiccator.

[0039] (4) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 40 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0040] (5) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.6Mpa to obtain a concentrated extract with a water content of 20%. 15% dextrin and 7% fructose by mass of the concentrated extract are added to it, and the stirring speed is 120r / min.

[0041] (6) Preparation of wetting conditioning solution: Prepare 3 parts of water and heat to 40°C. First, add 0.5 parts of ethanol, 0.6 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30. Then, heat to 50°C and add 0.4 parts of spermidine trihydrochloride.

[0042] (7) Crushing: After the above powder is stirred for 25 minutes, the wetting and conditioning solution is sprayed in 4 times. After stirring for 6 minutes, it is transferred to an air jet mill with an air flow rate of 400 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0043] Example 2

[0044] The model of the air jet mill is QL20. The specific steps are as follows:

[0045] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 20 parts of Cordyceps militaris powder and add 500 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 2 hours, then water bath at 50℃, ultrasonic power of 500w, treatment time of 50min, and then centrifuge and filter at 3000r / min to obtain Cordyceps militaris extract;

[0046] (2) Immobilization of cellulose microspheres as initiators: Take 0.6 parts of cellulose microspheres and wash them ultrasonically for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 6 parts of methyl pyruvate, 5 parts of TEA, 0.16 parts of DMAP and 0.25 parts of THF. Stir at 100 r / min and react in a constant temperature oil bath at 25℃ for 24 h. After the reaction, wash the cellulose microspheres ultrasonically three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then, vacuum dry them at 40℃ for 24 h and store them in a desiccator.

[0047] (3) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 20 parts of anisole, 25 parts of 1-(4-aminobenzyl)imidazol, 0.09 parts of methyl pyruvate, 0.01 CuBr2, and 0.12 PMDETA. After the addition is completed, bubbling with N2 for 15 min, constant temperature water bath at 30℃, react for 4 h, add 30 parts of dichloromethane to dilute, centrifuge and filter out the cellulose microspheres, and ultrasonically wash twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol respectively. After washing, the grafted microspheres are vacuum dried at 40℃ for 24 h and stored in a desiccator.

[0048] (4) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 50 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0049] (5) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.8Mpa to obtain a concentrated extract with a water content of 20%. 20% dextrin and 6% fructose by mass of the concentrated extract are added to it, and the stirring speed is 140r / min.

[0050] (6) Preparation of wetting conditioning solution: Prepare 2 parts of water and heat to 40°C. First, add 0.8 parts of ethanol, 0.5 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30. Then, heat to 50°C and add 0.5 parts of spermidine trihydrochloride.

[0051] (7) Crushing: After the above powder is stirred for 30 minutes, the wetting and conditioning solution is sprayed in 3 times. After stirring for 8 minutes, it is transferred to an air jet mill with an air flow rate of 300 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0052] Example 3

[0053] The model of the air jet mill is QL20. The specific steps are as follows:

[0054] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 25 parts of Cordyceps militaris powder and add 400 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 1 hour, then water bath at 50℃, ultrasonic power of 500w, treatment time of 40min, and then centrifuge and filter at 3000r / min to obtain Cordyceps militaris extract;

[0055] (2) Immobilization of cellulose microspheres as initiators: Take 0.8 parts of cellulose microspheres and wash them ultrasonically for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 8 parts of methyl pyruvate, 3 parts of TEA, 0.2 parts of DMAP and 0.2 parts of THF. Stir at 100 r / min and react in a constant temperature oil bath at 25℃ for 24 h. After the reaction, wash the cellulose microspheres ultrasonically three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then, vacuum dry them at 40℃ for 24 h and store them in a desiccator.

[0056] (3) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 25 parts of anisole, 20 parts of 1-(4-aminobenzyl)imidazolium, 0.15 parts of methyl pyruvate, 0.02 CuBr2, and 0.08 PMDETA. After the feeding is completed, N2 is bubbled for 15 min, and the mixture is kept in a constant temperature water bath at 30℃. After reacting for 4 h, 40 parts of dichloromethane are added for dilution. The cellulose microspheres are centrifuged and filtered out. They are ultrasonically washed twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol, respectively. The washed grafted microspheres are vacuum dried at 40℃ for 24 h and stored in a desiccator.

[0057] (4) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 30 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0058] (5) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.4Mpa to obtain a concentrated extract with a water content of 20%. 10% dextrin and 9% fructose by mass of the concentrated extract are added to it, and the stirring speed is 100r / min.

[0059] (6) Preparation of wetting conditioning solution: Prepare 5 parts of water and heat to 40°C. First, add 0.8 parts of ethanol, 0.8 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30. Then, heat to 50°C and add 0.3 parts of spermidine trihydrochloride.

[0060] (7) Crushing: After the above powder is stirred for 20 minutes, the wetting and conditioning solution is sprayed in 5 times. After stirring for 5 minutes, it is transferred to an air jet mill with an air flow rate of 500 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0061] Comparative Example 1

[0062] The air jet mill is model QL20. The difference between this comparative example and Example 1 is that the extraction process of Cordyceps militaris is hot water extraction combined with ultrasonic extraction. The specific steps are as follows:

[0063] Take dried Cordyceps militaris, pulverize it, and pass it through an 80-mesh sieve. Take 22 parts of Cordyceps militaris powder, add distilled water at a material-to-liquid ratio of 1:20, mix well, and after it is completely soaked, extract by ultrasonic crushing with an ultrasonic power of 500W for 45 minutes. Then, extract in a 90℃ constant temperature water bath for 2 hours, centrifuge and collect the filtrate. Repeat the above operation twice to obtain Cordyceps militaris extract. The remaining implementation methods are the same as in Example 1.

[0064] Comparative Example 2

[0065] The model of the air jet mill is QL20. The difference between this comparative example and Example 1 is that the sodium R-3-hydroxybutyrate in step (1) is EDTA. The rest of the implementation method is the same as Example 1.

[0066] Comparative Example 3

[0067] The model of the air jet mill is QL20. The difference between this comparative example and Example 1 is that in step (1), 450 parts of a mixed solution with a mass ratio of cellulase to water of 1:20 are added for 1.5 hours of enzymatic hydrolysis. The rest of the implementation method is the same as Example 1.

[0068] Comparative Example 4

[0069] The model of the air jet mill is QL20. The difference between this comparative example and Example 1 is that in step (1), 450 parts of a mixed solution with a mass ratio of cellulase: complexing agent: water of 1:0.5:20 are added for 1.5 hours of enzymatic hydrolysis. The rest of the implementation method is the same as Example 1.

[0070] Comparative Example 5

[0071] The model of the air jet mill is QL20. The specific steps are as follows:

[0072] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 22 parts of Cordyceps militaris powder and add 450 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 1.5 h, then water bath at 50 ℃, ultrasonic power of 500 W, treatment time of 45 min, and then centrifuge and filter at 3000 r / min to obtain Cordyceps militaris extract;

[0073] (2) Preparation of cellulose microspheres: 50 parts of NaOH:urea:distilled water in a mass ratio of 7:12:80 were mixed with 25 parts of cotton linter pulp with a degree of polymerization of 500. The resulting cellulose solution was then refrigerated at 8°C. 14 parts of polyoxyethylene ether and 52 parts of polyethylene glycol 1000 were mixed and stirred for 1 hour. The cellulose solution was then added dropwise to the polyethylene glycol solution while the water bath temperature was controlled at 45°C. After the addition was completed, the mixture was stirred for another 2 hours. Then, 37% dilute hydrochloric acid was added dropwise to the container until the system was neutral. Stirring was stopped, and the mixture was allowed to stand and separate into layers to obtain cellulose microspheres.

[0074] (3) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with cellulose microspheres at a ratio of 10:1, and adsorbed for 40 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0075] (4) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.6Mpa to obtain a concentrated extract with a water content of 20%. 15% dextrin and 7% fructose by mass of the concentrated extract are added to it, and the stirring speed is 120r / min.

[0076] (5) Preparation of wetting conditioning solution: Prepare 3 parts of water and heat to 40°C. First, add 0.5 parts of ethanol, 0.6 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30. Then, heat to 50°C and add 0.4 parts of spermidine trihydrochloride.

[0077] (6) Crushing: After the above powder is stirred for 25 minutes, the wetting and conditioning solution is sprayed in 4 times. After stirring for 6 minutes, it is transferred to an air jet mill with an air flow rate of 400 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0078] Comparative Example 6

[0079] The model of the air jet mill is QL20. The specific steps are as follows:

[0080] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 22 parts of Cordyceps militaris powder and add 450 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 1.5 h, then water bath at 50 ℃, ultrasonic power of 500 W, treatment time of 45 min, and then centrifuge and filter at 3000 r / min to obtain Cordyceps militaris extract;

[0081] (2) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was added dropwise into a polar macroporous adsorption resin containing nitrogen, oxygen and sulfur polar functional groups. The length and diameter of the resin column were 1000 mm and 100 mm, respectively. The elution flow rate was controlled at 3 ml / min. The filtrate was collected by filtration.

[0082] (3) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.6Mpa to obtain a concentrated extract with a water content of 20%. 15% dextrin and 7% fructose by mass of the concentrated extract are added to it, and the stirring speed is 120r / min.

[0083] (4) Preparation of wetting conditioning solution: Prepare 3 parts of water and heat to 40°C. First, add 0.5 parts of ethanol, 0.6 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30. Then, heat to 50°C and add 0.4 parts of spermidine trihydrochloride.

[0084] (5) Crushing: After the above powder is stirred for 25 minutes, the wetting and conditioning solution is sprayed in 4 times. After stirring for 6 minutes, it is transferred to an air jet mill with an air flow rate of 400 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0085] Comparative Example 7

[0086] The model of the air jet mill is QL20. The specific steps are as follows:

[0087] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 22 parts of Cordyceps militaris powder and add 450 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 1.5 h, then water bath at 50 ℃, ultrasonic power of 500 W, treatment time of 45 min, and then centrifuge and filter at 3000 r / min to obtain Cordyceps militaris extract;

[0088] (2) Immobilization of cellulose microspheres as initiators: Take 0.7 parts of cellulose microspheres and wash them ultrasonically for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 7 parts of methyl pyruvate, 4 parts of TEA, 0.18 parts of DMAP and 0.22 parts of THF. React in a constant temperature oil bath at 25℃ for 24 h with magnetic stirring at 100 r / min. After the reaction, wash the cellulose microspheres ultrasonically three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then, vacuum dry them at 40℃ for 24 h and store them in a desiccator.

[0089] (3) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 22 parts of anisole, 12 parts of 1-(4-aminobenzyl)imidazolium, 0.02 parts of methyl pyruvate, 0.015 CuBr2, and 0.1 PMDETA. After the addition is completed, bubbling with N2 for 15 min, constant temperature water bath at 30℃, reaction for 4 h, add 35 parts of dichloromethane for dilution, centrifuge and filter out the cellulose microspheres, and ultrasonically wash twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol respectively. After washing, the grafted microspheres are vacuum dried at 40℃ for 24 h and stored in a desiccator.

[0090] (4) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 40 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0091] (5) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.6Mpa to obtain a concentrated extract with a water content of 20%. 15% dextrin and 7% fructose by mass of the concentrated extract are added to it, and the stirring speed is 120r / min.

[0092] (6) Preparation of wetting conditioning solution: Prepare 3 parts of water and heat to 40°C. First, add 0.5 parts of ethanol, 0.6 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30. Then, heat to 50°C and add 0.4 parts of spermidine trihydrochloride.

[0093] (7) Crushing: After the above powder is stirred for 25 minutes, the wetting and conditioning solution is sprayed in 4 times. After stirring for 6 minutes, it is transferred to an air jet mill with an air flow rate of 400 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0094] Comparative Example 8

[0095] The model of the air jet mill is QL20. The specific steps are as follows:

[0096] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 22 parts of Cordyceps militaris powder and add 450 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 1.5 h, then water bath at 50 ℃, ultrasonic power of 500 W, treatment time of 45 min, and then centrifuge and filter at 3000 r / min to obtain Cordyceps militaris extract;

[0097] (2) Immobilization of cellulose microspheres as initiators: Take 0.7 parts of cellulose microspheres and wash them ultrasonically for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 7 parts of methyl pyruvate, 4 parts of TEA, 0.18 parts of DMAP and 0.22 parts of THF. React in a constant temperature oil bath at 25℃ for 24 h with magnetic stirring at 100 r / min. After the reaction, wash the cellulose microspheres ultrasonically three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then, vacuum dry them at 40℃ for 24 h and store them in a desiccator.

[0098] (3) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 22 parts of anisole, 32 parts of 1-(4-aminobenzyl)imidazolium, 0.25 parts of methyl pyruvate, 0.015 CuBr2, and 0.1 PMDETA. After the addition is completed, N2 is bubbled for 15 min, and the mixture is kept in a constant temperature water bath at 30℃. After reacting for 4 h, 35 parts of dichloromethane are added for dilution. The cellulose microspheres are centrifuged and filtered out. They are ultrasonically washed twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol, respectively. The washed grafted microspheres are vacuum dried at 40℃ for 24 h and stored in a desiccator.

[0099] (4) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 40 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0100] (5) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.6Mpa to obtain a concentrated extract with a water content of 20%. 15% dextrin and 7% fructose by mass of the concentrated extract are added to it, and the stirring speed is 120r / min.

[0101] (6) Preparation of wetting conditioning solution: Prepare 3 parts of water and heat to 40°C. First, add 0.5 parts of ethanol, 0.6 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30. Then, heat to 50°C and add 0.4 parts of spermidine trihydrochloride.

[0102] (7) Crushing: After the above powder is stirred for 25 minutes, the wetting and conditioning solution is sprayed in 4 times. After stirring for 6 minutes, it is transferred to an air jet mill with an air flow rate of 400 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0103] Comparative Example 9

[0104] The model of the air jet mill is QL20. The difference between this comparative example and Example 1 is that the methyl pyruvate in steps (2) and (3) is 2-bromoisobutyryl bromide. The rest of the implementation methods are the same as in Example 1.

[0105] Comparative Example 10

[0106] The model of the air jet mill is QL20. The difference between this comparative example and Example 1 is that the 1-(4-aminobenzyl)imidazolium in step (3) is 3-aminopropyltrimethoxysilane. The rest of the implementation methods are the same as in Example 1.

[0107] Comparative Example 11

[0108] The model of the air jet mill is QL20. The difference between this comparative example and Example 1 is that the methyl pyruvate in steps (2) and (3) is 2-bromoisobutyryl bromide and the 1-(4-aminobenzyl)imidazolium is 3-aminopropyltrimethoxysilane. The rest of the implementation methods are the same as in Example 1.

[0109] Comparative Example 12

[0110] The model of the air jet mill is QL20. The difference between this comparative example and Example 1 is that the spermidine trihydrochloride in step (6) is dodecyl dimethylamine oxide. The rest of the implementation method is the same as Example 1.

[0111] Comparative Example 13

[0112] The model of the air jet mill is QL20. The specific steps are as follows:

[0113] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 22 parts of Cordyceps militaris powder and add 450 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 1.5 h, then water bath at 50 ℃, ultrasonic power of 500 W, treatment time of 45 min, and then centrifuge and filter at 3000 r / min to obtain Cordyceps militaris extract;

[0114] (2) Immobilization of cellulose microspheres as initiators: Take 0.7 parts of cellulose microspheres and wash them ultrasonically for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 7 parts of methyl pyruvate, 4 parts of TEA, 0.18 parts of DMAP and 0.22 parts of THF. React in a constant temperature oil bath at 25℃ for 24 h with magnetic stirring at 100 r / min. After the reaction, wash the cellulose microspheres ultrasonically three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then, vacuum dry them at 40℃ for 24 h and store them in a desiccator.

[0115] (3) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 22 parts of anisole, 22 parts of 1-(4-aminobenzyl)imidazol, 0.12 parts of methyl pyruvate, 0.015 CuBr2, and 0.1 PMDETA. After the addition is completed, bubbling with N2 for 15 min, constant temperature water bath at 30℃, react for 4 h, add 35 parts of dichloromethane to dilute, centrifuge and filter out the cellulose microspheres, and ultrasonically wash twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol respectively. After washing, the grafted microspheres are vacuum dried at 40℃ for 24 h and stored in a desiccator.

[0116] (4) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 40 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0117] (5) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.6Mpa to obtain a concentrated extract with a water content of 20%. 15% dextrin and 7% fructose by mass of the concentrated extract are added to it, and the stirring speed is 120r / min.

[0118] (6) Preparation of wetting conditioning solution: Prepare 3 parts of water and heat to 40°C. First add 0.5 parts of ethanol, 0.6 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30, and stir evenly to obtain the solution.

[0119] (7) Crushing: After the above powder is stirred for 25 minutes, the wetting and conditioning solution is sprayed in 4 times. After stirring for 6 minutes, it is transferred to an air jet mill with an air flow rate of 400 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0120] Comparative Example 14

[0121] The model of the air jet mill is QL20. The specific steps are as follows:

[0122] (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 22 parts of Cordyceps militaris powder and add 450 parts of a mixed solution with a mass ratio of cellulase: sodium R-3-hydroxybutyrate: water of 1:0.1:20. Perform enzymatic hydrolysis for 1.5 h, then water bath at 50 ℃, ultrasonic power of 500 W, treatment time of 45 min, and then centrifuge and filter at 3000 r / min to obtain Cordyceps militaris extract;

[0123] (2) Immobilization of cellulose microspheres as initiators: Take 0.7 parts of cellulose microspheres and wash them ultrasonically for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 7 parts of methyl pyruvate, 4 parts of TEA, 0.18 parts of DMAP and 0.22 parts of THF. React in a constant temperature oil bath at 25℃ for 24 h with magnetic stirring at 100 r / min. After the reaction, wash the cellulose microspheres ultrasonically three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then, vacuum dry them at 40℃ for 24 h and store them in a desiccator.

[0124] (3) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 22 parts of anisole, 22 parts of 1-(4-aminobenzyl)imidazol, 0.12 parts of methyl pyruvate, 0.015 CuBr2, and 0.1 PMDETA. After the addition is completed, bubbling with N2 for 15 min, constant temperature water bath at 30℃, react for 4 h, add 35 parts of dichloromethane to dilute, centrifuge and filter out the cellulose microspheres, and ultrasonically wash twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol respectively. After washing, the grafted microspheres are vacuum dried at 40℃ for 24 h and stored in a desiccator.

[0125] (4) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 40 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration.

[0126] (5) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of -0.6Mpa to obtain a concentrated extract with a water content of 20%. 15% dextrin and 7% fructose by mass of the concentrated extract are added to it, and the stirring speed is 120r / min.

[0127] (6) Preparation of wetting conditioning solution: Prepare 3 parts of water and heat to 40°C. First, add 0.5 parts of ethanol, 0.6 parts of sodium carboxymethyl starch, and 0.05 parts of polyvinylpyrrolidone K30. Then, heat to 50°C and add 0.9 parts of spermidine trihydrochloride.

[0128] (7) Crushing: After the above powder is stirred for 25 minutes, the wetting and conditioning solution is sprayed in 4 times. After stirring for 6 minutes, it is transferred to an air jet mill with an air flow rate of 400 m / min. The Cordyceps militaris powder is obtained when it flows out.

[0129] I. Determination of polysaccharide components of Cordyceps militaris extract, scavenging rate of hydroxyl radicals in Cordyceps militaris extract, and retention rate of adsorbed and purified polysaccharides.

[0130] 1) Determination of the content of polysaccharides in Cordyceps militaris:

[0131] Sample solution: For each example and comparative example, weigh 10 mg of Cordyceps militaris concentrated extract crude product and add an appropriate amount of ultrapure water to prepare a test solution with a concentration of 5.0 mg / mL.

[0132] Preparation of standard solutions: Accurately weigh 10 mg of each of the dextran (5.0 kDa, 11.6 kDa, 23.8 kDa, 48.6 kDa, 147.6 kDa, 273.0 kDa, 409.8 kDa, 667.8 kDa, 1000.0 kDa) standards and prepare a 10 mg / mL standard solution.

[0133] Column: TOSOH TSK gel G5000PWx L Chromatographic column (7.8 x 300 mm); mobile phase: 0.1 M NaSO4 solution, flow rate: 1.0 M / min; column temperature: 30 °C; injection volume: 20 L, column pressure: 1.8 MPa; detector: RID.

[0134] 2) Determination of the scavenging rate of hydroxyl free radicals in polysaccharide components:

[0135] Add 2 mL of 9 mmol / L FeSO4, 2 mL of 9 mmol / L salicylic acid, 2 mL of the test sample, and 2 mL of 8.8 mmol / L H2O2 sequentially to the test tube, shake well, and incubate in a water bath at 37°C for 30 min. The test sample is the Cordyceps militaris extract from Examples 1-3 and Comparative Examples 1-14.

[0136] The test sample in the test tube was replaced with an equal volume of distilled water in the control tube.

[0137] The absorbance of the test tube and the control tube was measured in a spectrophotometer with a wavelength of 447 nm.

[0138] Hydroxyl radical scavenging rate = (A0-A1) / A0 × 100%;

[0139] A0 represents the absorbance value of the control tube, and A1 represents the absorbance value of the test tube.

[0140] The scavenging rates of hydroxyl radicals in Examples 1-3 and Comparative Examples 1-14 were calculated according to the formula.

[0141] 3) Polysaccharide retention rate after adsorption purification = (p1 / p2) × 100%

[0142] P1 and p2 are the absorbance of the sample solution at 490 nm after the sulfuric acid-phenol method color development, before and after adsorption purification, respectively.

[0143] The results are shown in Table 1.

[0144] Table 1. Results of determination of polysaccharide components and hydroxyl radical scavenging rate of Cordyceps militaris.

[0145] Group Polysaccharide yield (%) Polysaccharide extraction rate (%) Hydroxyl radical scavenging capacity (%) Polysaccharide retention rate after adsorption purification (%) Example 1 23.77 73.68 91.72 87.41 Example 2 25.45 75.34 92.56 85.53 Example 3 24.45 72.77 91.85 86.97 Comparative Example 1 10.42 61.74 62.38 67.65 Comparative Example 2 21.89 70.54 75.14 68.52 Comparative Example 3 18.49 67.81 66.24 80.42 Comparative Example 4 17.65 66.92 67.13 79.56 Comparative Example 5 22.84 71.53 74.56 65.48 Comparative Example 6 23.54 71.68 65.42 61.81 Comparative Example 7 22.84 72.59 66.45 64.71 Comparative Example 8 23.65 72.32 67.19 67.36 Comparative Example 9 22.57 71.89 70.53 66.28 Comparative Example 10 22.94 71.20 67.86 69.48 Comparative Example 11 23.41 69.84 69.57 74.81 Comparative Example 12 23.68 69.51 71.41 78.51 Comparative Example 13 23.41 73.14 74.52 74.52 Comparative Example 14 24.10 73.62 77.23 76.47

[0146] II. Powder wettability test:

[0147] The wettability test was conducted as follows: 100±1 ml of 342 ppm hard water (0.304 g anhydrous calcium chloride and 0.139 g magnesium chloride hexahydrate diluted to 1 liter with distilled water) was poured into a 250 ml beaker. This beaker was placed in a constant temperature water bath at 25±1℃, with the liquid level flush with the water bath's surface. When the hard water reached 25±1℃, 5±0.1 g of sample was weighed using a watch glass. The entire sample was poured evenly onto the liquid surface of the beaker from a position flush with the rim, without excessively disturbing the liquid surface. A stopwatch was immediately started to time the process until the sample was completely wetted. The wetting time was recorded. This process was repeated three times, and the average value was taken as the wetting time of the sample. Wetting tests were performed on Examples 1-3 and Comparative Examples 1-7, and the results are shown in Table 2 below.

[0148] Table 2 Wettability Results

[0149] Group Wettability / s Example 1 68 Example 2 64 Example 3 72 Comparative Example 1 78 Comparative Example 2 79 Comparative Example 3 71 Comparative Example 4 73 Comparative Example 5 75 Comparative Example 6 70 Comparative Example 7 71 Comparative Example 8 73 Comparative Example 9 79 Comparative Example 10 75 Comparative Example 11 76 Comparative Example 12 78 Comparative Example 13 85 Comparative Example 14 88

Claims

1. A preparation process for Cordyceps militaris powder, characterized in that, Its preparation process is as follows: (1) Enzymatic hydrolysis and ultrasonic extraction of Cordyceps militaris: Take dried Cordyceps militaris, crush it and pass it through an 80-mesh sieve. Take 20-25 parts of Cordyceps militaris powder and add 400-500 parts of a mixed solution of cellulase, complexing agent and water in a certain mass ratio. Perform enzymatic hydrolysis for 1-2 hours. Then, use a water bath at 50℃ and ultrasonic power of 500w for 40-50 minutes. Then, centrifuge and filter at 3000r / min to obtain Cordyceps militaris extract. (2) Separation and purification of Cordyceps militaris extract: The above Cordyceps militaris extract was mixed with porous and highly adsorbent cellulose microspheres at a ratio of 10:1, and adsorbed for 30-50 min in a constant temperature shaker at 110 r / min and a 45℃ water bath. The filtrate was then collected by filtration. (3) Powder mixing: The filtrate after adsorption is concentrated at a temperature of 80℃ and a vacuum of (-0.8)-(-0.4) MPa to obtain a concentrated extract with a water content of 20%. 10%-20% of dextrin and 6%-9% of fructose by mass of the concentrated extract are added to it, and the stirring speed is 100-140 r / min. (4) Crushing: After the above powder is stirred for 20-30 minutes, spray 3.15-7.15 parts of wetting and conditioning solution in 3-5 times, continue stirring for 5-8 minutes, and then transfer it to an air jet mill with an air flow rate of 300-500 m / min. The Cordyceps militaris powder is obtained when it flows out. The complexing agent in step (1) is sodium R-3-hydroxybutyrate; The mass ratio of cellulase, complexing agent, and water in step (1) is 1:0.1:

20. The porous, highly absorbent cellulose microspheres in step (2) are prepared as follows: 1) Immobilization of cellulose microspheres with initiator: Take 0.6-0.8 parts of cellulose microspheres and ultrasonically wash them for 5 min each in 70% ethanol, 70% acetone and 70% THF solutions. Take out the washed cellulose microspheres and add 6-8 parts of initiator, 3-5 parts of TEA, 0.16-0.2 parts of DMAP and 0.2-0.25 parts of THF. React in a constant temperature oil bath at 25℃ for 24 h with magnetic stirring at 100 r / min. After reaction, ultrasonically wash the cellulose microspheres three times in 70% THF, 70% ethanol and 70% methanol solutions for 5 min each time. Then vacuum dry them at 40℃ for 24 h and store them in a desiccator. 2) ARGET ATRP grafting modification method: Take the cellulose microspheres immobilized by the above initiator, add 20-25 parts anisole, 20-25 parts grafting agent, 0.09-0.15 parts methyl pyruvate, 0.01-0.02 CuBr2, and 0.08-0.12 PMDETA. After the addition is complete, bubble with N2 for 15 min, and react in a constant temperature water bath at 30℃ for 4 h. Then add 30-40 parts dichloromethane to dilute, centrifuge and filter out the cellulose microspheres, and ultrasonically wash twice with 70% dichloromethane, 70% THF, 70% water, 70% methanol, and 70% ethanol respectively. After washing, vacuum dry the grafted microspheres at 40℃ for 24 h and store them in a desiccator. The initiator is methyl pyruvate; The grafting agent is 1-(4-aminobenzyl)imidazol.

2. The preparation process of Cordyceps militaris powder as described in claim 1, characterized in that: The wetting conditioning solution in step (4) is prepared as follows: Prepare 2-5 parts of water and heat it to 40°C. First, add 0.3-0.8 parts of ethanol, 0.5-0.8 parts of sodium carboxymethyl starch, and 0.05 parts of povidone K30. Then, heat it to 50°C and add the wetting conditioner.

3. The preparation process of Cordyceps militaris powder as described in claim 2, characterized in that: in, The wetting regulator is spermidine trihydrochloride.

4. The preparation process of Cordyceps militaris powder as described in claim 2, characterized in that: The wetting regulator is specifically 0.3-0.5 parts.