A cordyceps sinensis composition and a preparation method thereof

Abstract

The present application relates to a kind of cordyceps sinensis composition and its preparation method, the preparation method is simple, the effective component content of the composition obtained by the preparation method is high, the dissolution rate and dissolution rate of worm grass polysaccharide are high, stability is good, overall appearance and microscopic appearance are good, physical strength is big, disintegration speed is fast, not sticking oral cavity, with good mouth feel.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine preparation technology, and in particular to a Cordyceps sinensis composition and its preparation method. Background Technology

[0002] Fresh herbs have a long history of use and definite curative effects, but they are prone to rotting and mold, and are difficult to store and transport, which seriously restricts their application and development. Fresh herbs are also difficult to process, and at present there are very few fresh herb preparations available, which are insufficient to meet market demand.

[0003] Traditional methods of applying fresh medicinal herbs mainly include internal administration through juice extraction, external application through crushing, and decoction. These methods are not only inconvenient but also difficult to obtain due to seasonal and geographical limitations. Most of the active ingredients in Chinese medicinal herbs are distributed within cells. Fresh herbs have intact cell structures, and using traditional decoction methods, the utilization rate of active ingredients is only 10%-30%, which is very limited. However, by using appropriate technology to prepare fresh herbs into cell-wall-broken slices, the dissolution of active ingredients can be improved, greatly enhancing their efficacy, with an effective ingredient utilization rate exceeding 90%. Cell-wall-broken slices can significantly improve the dissolution of active ingredients and enhance efficacy. However, because fresh herbs contain a large amount of water, and some herbs have high levels of polysaccharides, oils, and other viscous components, if industry-standard cell-wall-breaking technologies such as ultrafine pulverizers or air jet mills are used, the herbal powder will clump together, adhere to the vibrating bar, and clog the discharge port, making it impossible to pulverize and break down the cell walls.

[0004] Traditional medicinal herbs require long cooking times and cannot be cooked in metal utensils, which limits their use in many ways. The industry has also conducted research on this issue and has achieved some results in innovative medicinal herbs, such as Chinese herbal formula granules. However, fresh herbs have not yet been involved, and Chinese herbal formula granules have been questioned due to the potential loss of medicinal components.

[0005] Therefore, there is still an urgent need for a fresh herb composition that is convenient and easy to take, has good dissolution effect, and high content of active ingredients, as well as its preparation method. Summary of the Invention

[0006] To address the above problems, the present invention provides a composition and a method for preparing the same.

[0007] In a first aspect, the present invention provides a method for preparing a composition.

[0008] A method for preparing a composition includes: taking medicinal materials, adding water to homogenize and pulverize, wet ball milling, freeze drying to obtain the composition, wherein the freeze drying includes pre-freezing, sublimation drying and desorption drying, and the pre-freezing is performed by gradient cooling.

[0009] The weight percentage of the medicinal material in the total weight of water and medicinal material can be 7 wt% to 30 wt%. In some embodiments, the weight percentage of the medicinal material in the total weight of water and medicinal material is 10 wt% to 15 wt%.

[0010] The pre-freezing parameters can be as follows: Pre-freezing stage 1: Adjust the temperature to -10℃ to -5℃ within 20-40 minutes and maintain this temperature for 60 min to 600 min, with a pressure of 0.09 MPa to 0.11 MPa; Pre-freezing stage 2: Adjust the temperature to -25℃ to -15℃ within 20-40 minutes and maintain this temperature for 60 min to 600 min, with a pressure of 0.09 MPa to 0.11 MPa; and Pre-freezing stage 3: Adjust the temperature to -40℃ to -35℃ within 20-40 minutes and maintain this temperature for 60 min to 600 min, with a pressure of 0.09 MPa to 0.11 MPa.

[0011] In some embodiments, the pre-freezing parameters are as follows: Pre-freezing stage 1: adjusting the temperature to -5°C within 30 minutes and maintaining this temperature for 120 minutes, with a pressure of 0.09 MPa to 0.11 MPa; Pre-freezing stage 2: adjusting the temperature to -20°C within 30 minutes and maintaining this temperature for 120 minutes, with a pressure of 0.09 MPa to 0.11 MPa; and Pre-freezing stage 3: adjusting the temperature to -40°C within 20-40 minutes and maintaining this temperature for 120 minutes, with a pressure of 0.09 MPa to 0.11 MPa.

[0012] The parameters for the sublimation drying can be: adjusting the temperature to -10℃ to -5℃ within 45 to 100 minutes, maintaining this temperature for 1000 to 3000 minutes, and the pressure being 10 Pa to 50 Pa. In some embodiments, the parameters for the sublimation drying are: adjusting the temperature to -5℃ within 60 minutes, maintaining this temperature for 1500 minutes, and the pressure being 13 Pa to 30 Pa.

[0013] The parameters for the analytical drying can be: adjusting the temperature to 20°C to 30°C within 20-40 minutes and maintaining this temperature for 200-600 minutes, with a pressure of 10 Pa to 50 Pa. In some embodiments, the parameters for the sublimation drying are: adjusting the temperature to 25°C within 30 minutes and maintaining this temperature for 360 minutes, with a pressure of 13 Pa to 30 Pa.

[0014] The particle size of the medicinal powder obtained after wet ball milling can be D90≤45μm.

[0015] The operation steps of the wet ball milling are as follows: take ball milling beads with a particle size of 0.1 mm to 5 mm and ball mill them with the homogenized slurry. The weight of the ball milling beads is 1 to 5 times the weight of the homogenized slurry. The ball milling time is 30 min to 90 min.

[0016] In some embodiments, the grinding beads have a particle size of 0.5-2 mm. In some embodiments, the grinding beads have a particle size of 0.5-1 mm. In some embodiments, the grinding beads have a particle size of 0.8 mm.

[0017] In some embodiments, the weight of the grinding beads is 1-4 times the weight of the homogenized slurry. In some embodiments, the weight of the grinding beads is 2-4 times the weight of the homogenized slurry. In some embodiments, the weight of the grinding beads is 3 times the weight of the homogenized slurry.

[0018] In some embodiments, the ball milling time is 60 minutes.

[0019] In some embodiments, the operation steps of the wet ball milling are as follows: take ball milling beads with a particle size of 0.5 mm to 2 mm and ball mill them with the homogenized slurry. The weight of the ball milling beads is 1 to 4 times the weight of the homogenized slurry. The ball milling time is 30 min to 90 min.

[0020] In some embodiments, the operation steps of the wet ball milling are as follows: take ball milling beads with a particle size of 0.5 mm to 1 mm and ball mill them with the homogenized slurry. The weight of the ball milling beads is 2 to 4 times the weight of the homogenized slurry. The ball milling time is 30 min to 60 min.

[0021] In some embodiments, the operation steps of the wet ball milling are as follows: take ball milling beads with a particle size of 0.8 mm and ball mill the homogenized slurry, the weight of the ball milling beads is 3 times the weight of the homogenized slurry, and the ball milling time is 60 min.

[0022] In some embodiments, the medicinal material may be a fresh medicinal material. In some embodiments, the medicinal material is Cordyceps sinensis. In some embodiments, the medicinal material is dried Cordyceps sinensis or fresh Cordyceps sinensis.

[0023] In a second aspect, the present invention provides a composition prepared by the method described in the first aspect.

[0024] A composition prepared by the method described in the first aspect.

[0025] The composition described in the first or second aspect can be a direct-drinking tablet; the direct-drinking tablet can be taken orally or dissolved in water.

[0026] Beneficial effects

[0027] Compared with the prior art, the present invention has the following beneficial technical effects:

[0028] (1) The freeze-dried direct-drinking slices obtained by the present invention through wet ball milling combined with gradient cooling pre-freezing retain the "fresh" characteristics. In addition, compared with the preparation method using ultrafine pulverization or single-temperature pre-freezing, the freeze-dried direct-drinking slices obtained by ball milling cell wall breaking combined with gradient cooling can greatly increase the content of Cordyceps polysaccharides and medicinal amino acids, especially the content of methionine is increased by nearly 100%, and the content of functional amino acids such as aspartic acid, glutamic acid, tyrosine, phenylalanine, leucine and lysine are all significantly increased.

[0029] (2) Compared with the preparation method of ultra-fine pulverization or single temperature pre-freezing, the freeze-dried direct-drinking slices of fresh Cordyceps sinensis obtained by ball milling and gradient cooling can greatly improve the dissolution rate and dissolution degree of Cordyceps polysaccharides, and greatly improve the effective utilization of precious medicinal materials.

[0030] (3) Neither wet ball milling nor gradient cooling pre-freezing alone can improve the stability of superoxide dismutase activity in freeze-dried direct-drinking slices of fresh Cordyceps sinensis. However, the present invention, by combining wet ball milling and gradient cooling pre-freezing, can greatly improve the stability of superoxide dismutase activity in freeze-dried direct-drinking slices of fresh Cordyceps sinensis, achieving a synergistic effect and unexpected technical results.

[0031] (4) Neither wet ball milling nor gradient cooling pre-freezing alone can produce freeze-dried cakes with high physical strength, which are not easily broken, can quickly absorb water and disintegrate after contact with water, and are not easily adhered to the inner wall of the mouth. However, the freeze-dried direct-drinking slices prepared by combining wet ball milling and gradient cooling pre-freezing in this invention can produce freeze-dried direct-drinking slices with a neat and flat overall appearance, a three-dimensional network structure in microscopic appearance, high physical strength, which are not easily broken, can quickly absorb water and disintegrate after contact with water, and are not easily adhered to the inner wall of the mouth.

[0032] (5) Compared with freeze-dried direct-drinking slices obtained by wet ball milling or gradient cooling pre-freezing alone, the freeze-dried direct-drinking slices prepared by combining wet ball milling and gradient cooling pre-freezing in this invention can retain the flavor of fresh medicinal materials very well. Moreover, it has a sponge-like structure, a large specific surface area, is easily dissolved by the oral mucosa, does not adhere to the oral cavity, and has no grainy feel.

[0033] Terminology Explanation

[0034] In this invention, "wt%" represents weight percentage. "MPa" represents the pressure unit "megapascal". "Pa" represents the pressure unit "pascal". Attached Figure Description

[0035] Figure 1 The image shows the overall appearance of the freeze-dried Cordyceps sinensis slices obtained in Example 1.

[0036] Figure 2 This is a partial enlarged side view of the freeze-dried Cordyceps sinensis slices obtained in Example 1.

[0037] Figure 3 This is a partially enlarged cross-sectional view of the freeze-dried Cordyceps sinensis slices obtained in Example 1.

[0038] Figure 4 This is a partially enlarged longitudinal section of the freeze-dried Cordyceps sinensis slices obtained in Example 1.

[0039] Figure 5 The image shows the overall appearance of the freeze-dried Cordyceps sinensis slices obtained in Example 2.

[0040] Figure 6 This is a partial enlarged side view of the freeze-dried Cordyceps sinensis slices obtained in Example 2.

[0041] Figure 7 This is a partially enlarged cross-sectional view of the freeze-dried Cordyceps sinensis slices obtained in Example 2.

[0042] Figure 8 This is a partially enlarged longitudinal section of the freeze-dried Cordyceps sinensis slices obtained in Example 2.

[0043] Figure 9 The image shows the overall appearance of the freeze-dried Cordyceps sinensis slices obtained in Example 3.

[0044] Figure 10 This is a partial enlarged side view of the freeze-dried Cordyceps sinensis slices obtained in Example 3.

[0045] Figure 11 This is a partially enlarged cross-sectional view of the freeze-dried Cordyceps sinensis slices obtained in Example 3.

[0046] Figure 12 This is a partially enlarged longitudinal section of the freeze-dried Cordyceps sinensis slices obtained in Example 3.

[0047] Figure 13 The image shows the overall appearance of the freeze-dried Cordyceps sinensis slices obtained in Example 4.

[0048] Figure 14 This is a partial enlarged side view of the freeze-dried Cordyceps sinensis slices obtained in Example 4.

[0049] Figure 15 This is a partially enlarged cross-sectional view of the freeze-dried Cordyceps sinensis slices obtained in Example 4.

[0050] Figure 16This is a partially enlarged longitudinal section of the freeze-dried Cordyceps sinensis slices obtained in Example 4.

[0051] Figure 17 The image shows the overall appearance of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 1.

[0052] Figure 18 This is a magnified side view of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 1.

[0053] Figure 19 This is a magnified cross-section of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 1.

[0054] Figure 20 This is a magnified longitudinal section of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 1.

[0055] Figure 21 The image shows the overall appearance of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 2.

[0056] Figure 22 This is a magnified side view of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 2.

[0057] Figure 23 This is a magnified cross-section of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 2.

[0058] Figure 24 This is a magnified longitudinal section of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 2.

[0059] Figure 25 The image shows the overall appearance of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 3.

[0060] Figure 26 This is a magnified side view of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 3.

[0061] Figure 27 This is a magnified cross-section of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 3.

[0062] Figure 28 This is a partially enlarged longitudinal section of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 3.

[0063] Figure 29 The image shows the overall appearance of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 4.

[0064] Figure 30 This is a magnified side view of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 4.

[0065] Figure 31This is a magnified cross-section of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 4.

[0066] Figure 32 This is a magnified longitudinal section of the freeze-dried Cordyceps sinensis slices obtained in Comparative Example 4. Detailed Implementation

[0067] To enable those skilled in the art to better understand the technical solutions of the present invention, some non-limiting embodiments are further disclosed below to provide a more detailed description of the present invention.

[0068] All reagents used in this invention can be purchased commercially or prepared by the methods described in this invention.

[0069] Example 1: Preparation of freeze-dried fresh Cordyceps sinensis slices for direct consumption

[0070] Prepare freeze-dried direct-drinking slices of fresh Cordyceps sinensis according to the following steps:

[0071] 1. Cleaning: Select fresh Cordyceps sinensis, remove the outer fungal film and impurities such as dirt, rinse with pure running water, place in a sieve and let it drain in a cool place for later use;

[0072] 2. Grinding: Take 100g of Cordyceps sinensis after cleaning in step 1, add 300g of purified water, and homogenize and grind it using a homogenizer; obtain a homogenate. Take the homogenate and 3 times the weight of the homogenate and 0.5mm zirconium dioxide ball milling beads and grind them together in a ball mill jar for 60min to make the particle size D90≤45μm. Separate to obtain fresh Cordyceps sinensis cell wall broken pulp.

[0073] 3. Freeze-drying: The cell wall-breaking slurry obtained in step 2 is filled into vials at a rate of 250 mg Cordyceps sinensis per vial, and freeze-dried according to the following freeze-drying process parameters to obtain freeze-dried direct-drinking slices of fresh Cordyceps sinensis:

[0074]

[0075]

[0076] Example 2: Preparation of freeze-dried fresh Cordyceps sinensis slices for direct consumption

[0077] 1. Cleaning: Select fresh Cordyceps sinensis, remove the outer fungal film and impurities such as dirt, rinse with pure running water, place in a sieve and let it drain in a cool place for later use.

[0078] 2. Pulverization: Take 100g of Cordyceps sinensis after cleaning in step 1, add 1400g of purified water, and homogenize and pulverize it using a homogenizer; obtain a homogenate. Take the homogenate and 5 times the weight of the homogenate and 2mm zirconia ball milling beads and put them into a ball mill jar and grind for 30min to make the particle size D90≤45μm. Separate to obtain fresh Cordyceps sinensis cell wall broken pulp.

[0079] 3. Freeze-drying: The cell wall-breaking slurry obtained in step 2 is filled into vials at a rate of 250 mg Cordyceps sinensis per vial, and freeze-dried according to the following freeze-drying process parameters to obtain freeze-dried direct-drinking slices of fresh Cordyceps sinensis:

[0080]

[0081] Example 3: Preparation of freeze-dried fresh Cordyceps sinensis slices for direct consumption

[0082] 1. Cleaning: Select fresh Cordyceps sinensis, remove the outer fungal film and impurities such as dirt, rinse with pure running water, place in a sieve and let it drain in a cool place for later use.

[0083] 2. Grinding: Take 100g of Cordyceps sinensis after cleaning in step 1, add 333g of purified water, and homogenize and grind it using a homogenizer; obtain a homogenate. Take the homogenate and zirconia ball milling beads with a particle size of 0.8mm (equal to the weight of the homogenate) and grind them together in a ball mill jar for 90min to make the particle size D90≤45μm. Separate to obtain fresh Cordyceps sinensis cell wall broken pulp.

[0084] 3. Freeze-drying: The cell wall-breaking slurry obtained in step 2 is filled into vials at a rate of 250 mg Cordyceps sinensis per vial, and freeze-dried according to the following freeze-drying process parameters to obtain freeze-dried direct-drinking slices of fresh Cordyceps sinensis:

[0085]

[0086] Example 4: Preparation of freeze-dried Cordyceps sinensis slices for direct consumption

[0087] 1. Pulverization: Take 100g of dried Cordyceps sinensis, add 900g of purified water, and homogenize and pulverize using a homogenizer; obtain a homogenate, take the homogenate and 3 times the weight of the homogenate and 0.8mm zirconium dioxide ball milling beads, put them into a ball mill jar and grind for 90min to make the particle size D90≤45μm, separate, and obtain the dried Cordyceps sinensis cell wall broken slurry;

[0088] 2. Freeze-drying: The cell wall-breaking slurry obtained in step 1 is filled into vials at a rate of 250 mg Cordyceps sinensis per vial, and freeze-dried according to the following freeze-drying process parameters to obtain freeze-dried Cordyceps sinensis slices for direct consumption:

[0089]

[0090] Comparative Example 1: Preparation of freeze-dried fresh Cordyceps sinensis slices for direct consumption (ultrafine grinding)

[0091] 1. Cleaning: Select fresh Cordyceps sinensis, remove the outer fungal film and impurities such as dirt, rinse with pure running water, place in a sieve and let it drain in a cool place for later use.

[0092] 2. Pulverization: Take 100g of Cordyceps sinensis washed in step 1, dry it and then pulverize it with an ultra-micro pulverizer until it passes through a 100-mesh sieve (D90>45μm). Add 300g of purified water and homogenize it with a homogenizer to obtain a fresh Cordyceps sinensis homogenate.

[0093] 3. Freeze-drying: The homogenate obtained in step 2 is filled into vials at a rate of 250 mg Cordyceps sinensis per vial, and then freeze-dried according to the following freeze-drying process parameters to obtain freeze-dried direct-drinking slices of fresh Cordyceps sinensis:

[0094]

[0095] Comparative Example 2: Preparation of freeze-dried fresh Cordyceps sinensis slices for direct consumption (investigation of pre-freezing temperature)

[0096] 1. Cleaning: Select fresh Cordyceps sinensis, remove the outer fungal film and impurities such as dirt, rinse with pure running water, place in a sieve and let it drain in a cool place for later use.

[0097] 2. Pulverization: Take 100g of Cordyceps sinensis after cleaning in step 1, add 300g of purified water, and homogenize and pulverize it using a homogenizer; take the homogenate and 3 times the weight of the homogenate and 0.5mm zirconium dioxide ball milling beads and grind them together in a ball mill jar for 60min to make the particle size D90≤45μm, and separate to obtain fresh Cordyceps sinensis cell wall broken pulp;

[0098] 3. Freeze-drying: The cell wall-breaking slurry obtained in step 2 is filled into vials at a rate of 250mg Cordyceps sinensis per vial, and freeze-dried according to the following freeze-drying process parameters to obtain freeze-dried direct-drinking slices of fresh Cordyceps sinensis:

[0099] step Temperature / °C Adjust time / min Hold time / min pressure Pre-freezing -40 30 360 0.10MPa Sublimation drying -5 60 1500 13Pa Analysis and drying 25 30 360 13Pa

[0100] Comparative Example 3: Preparation of freeze-dried fresh Cordyceps sinensis slices for direct consumption (investigation of pre-freezing temperature)

[0101] 1. Cleaning: Select fresh Cordyceps sinensis, remove the outer fungal film and impurities such as dirt, rinse with pure running water, place in a sieve and let it drain in a cool place for later use.

[0102] 2. Pulverization: Take 100g of cleaned Cordyceps sinensis from step 1, add 300g of purified water, and homogenize and pulverize using a homogenizer; take the homogenate and 3 times the weight of the homogenate and 0.5mm zirconium dioxide ball milling beads and grind them together in a ball mill jar for 60min to make the particle size D90≤45μm, and separate to obtain fresh Cordyceps sinensis cell wall broken pulp;

[0103] 3. Freeze-drying: The cell wall-breaking slurry obtained in step 2 is filled into vials at a rate of 250mg Cordyceps sinensis per vial, and freeze-dried according to the following freeze-drying process parameters to obtain freeze-dried direct-drinking slices of fresh Cordyceps sinensis:

[0104]

[0105]

[0106] Comparative Example 4: Preparation of freeze-dried fresh Cordyceps sinensis slices for direct consumption (investigation of pre-freezing temperature)

[0107] 1. Cleaning: Select fresh Cordyceps sinensis, remove the outer fungal film and impurities such as dirt, rinse with pure running water, place in a sieve and let it drain in a cool place for later use.

[0108] 2. Pulverization: Take 100g of cleaned Cordyceps sinensis from step 1, add 300g of purified water, and homogenize and pulverize using a homogenizer; take the homogenate and 3 times the weight of the homogenate and 0.5mm zirconium dioxide ball milling beads and grind them together in a ball mill jar for 60min to make the particle size D90≤45μm, and separate to obtain fresh Cordyceps sinensis cell wall broken pulp;

[0109] 3. Freeze-drying: The cell wall-breaking slurry obtained in step 2 is filled into vials at a rate of 250mg Cordyceps sinensis per vial, and freeze-dried according to the following freeze-drying process parameters to obtain freeze-dried direct-drinking slices of fresh Cordyceps sinensis:

[0110] step Temperature / °C Adjust time / min Hold time / min pressure Pre-freezing -20 30 360 0.10MPa Sublimation drying -5 60 1500 13Pa Analysis and drying 25 30 360 13Pa

[0111] Example 5: Detection of active ingredient content

[0112] The main active ingredients in Cordyceps sinensis are cordyceps polysaccharides, superoxide dismutase (SOD), and medicinal amino acids. Freeze-dried direct-drinking slices of fresh Cordyceps sinensis obtained in Example 1 and Comparative Examples 1-2 were used. The activity of superoxide dismutase (SOD) was tested according to GB / T 5009.171-2003 "Determination of Superoxide Dismutase (SOD) Activity in Health Foods," and the amino acid content was tested according to GB5009.124-2016 "National Food Safety Standard - Determination of Amino Acids in Foods." Cordyceps polysaccharides were detected using the phenol-sulfuric acid method. The results are shown in Table 1.

[0113] Table 1: Determination of the effective components of freeze-dried direct-drinking slices

[0114]

[0115]

[0116] Conclusion: Comparing Example 1, Comparative Example 1, and Comparative Example 2, it was found that Example 1 better preserved the activity of superoxide dismutase in Cordyceps sinensis, indicating that the freeze-dried direct-drinking slices obtained by pre-freezing fresh Cordyceps sinensis using wet ball milling combined with gradient cooling still retain the "fresh" characteristics. Furthermore, compared with preparation methods using ultrafine pulverization or single-temperature pre-freezing, the freeze-dried direct-drinking slices obtained by ball milling combined with gradient cooling significantly increased the content of Cordyceps polysaccharides and medicinal amino acids, especially methionine, which increased by nearly 100%. The contents of functional amino acids such as aspartic acid, glutamic acid, tyrosine, phenylalanine, leucine, and lysine also showed significant increases.

[0117] Example 6: Dissolution detection of Cordyceps polysaccharides

[0118] The freeze-dried direct-drinking slices of fresh Cordyceps sinensis obtained in Example 1 and Comparative Examples 1-4 were tested according to the third method of "0931 Determination of Dissolution and Release" in the General Chapter of Part IV of the 2020 Chinese Pharmacopoeia. The results are shown in Table 2.

[0119] Table 2: Cordyceps polysaccharide dissolution data

[0120]

[0121]

[0122] Conclusion: Comparing the 60-minute dissolution rate of Cordyceps polysaccharides in Example 1, Comparative Example 1, Comparative Example 2, Comparative Example 3, and Comparative Example 4, it was found that Example 1 can effectively improve the dissolution rate of Cordyceps polysaccharides in freeze-dried direct-drinking slices of fresh Cordyceps sinensis. This indicates that compared with preparation methods using ultrafine pulverization or single-temperature pre-freezing, the freeze-dried direct-drinking slices of fresh Cordyceps sinensis obtained by ball milling combined with gradient cooling can greatly improve the dissolution rate and dissolution rate of Cordyceps polysaccharides, thus greatly improving the effective utilization of this precious medicinal material.

[0123] Example 7: Detection of accelerated stability of superoxide dismutase activity

[0124] Freeze-dried decoction pieces of fresh Cordyceps sinensis obtained in Example 1 and Comparative Examples 1-4 were subjected to accelerated stability testing under accelerated conditions (40℃, 75% RH) for three months according to the accelerated testing method in the General Chapter "9001 Stability Testing Guidelines for Raw Materials and Preparations" of the 2020 edition of the Chinese Pharmacopoeia (Part IV). The superoxide dismutase activity of the samples was detected, and the results are shown in Table 3.

[0125] Table 3 Comparison of accelerated stability superoxide dismutase activity

[0126] Accelerated Months Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Example 1 0 11674.1 U / g 12763.8 U / g 12943.4 U / g 13276.9 U / g 15045.7 U / g 1 8013.7U / g 8435.2 U / g 9024.0 U / g 9458.7 U / g 11284.3 U / g 2 3974.2 U / g 4029.6 U / g 4516.4 U / g 4961.4 U / g 8127.9 U / g 3 2042.5 U / g 2384.7 U / g 2561.8 U / g 2843.4 U / g 6257.1 U / g

[0127] Conclusion: As shown in Table 3, in the three-month accelerated stability test, the superoxide dismutase (SOD) activity of freeze-dried Cordyceps sinensis slices from Examples 1, 1, 2, 3, and 4 decreased by 58.4%, 82.5%, 81.3%, 80.2%, and 78.6%, respectively. The results indicate that the preparation process of Example 1 can slow down the rate of decrease in SOD activity, proving that neither wet ball milling nor gradient cooling pre-freezing alone can improve the stability of SOD activity in freeze-dried Cordyceps sinensis slices. However, the combination of wet ball milling and gradient cooling pre-freezing significantly improves the stability of SOD activity in freeze-dried Cordyceps sinensis slices, exhibiting a synergistic effect and demonstrating unexpected technical advantages.

[0128] Example 8: Appearance and microstructure of freeze-dried direct-drinking beverage slices

[0129] Freeze-dried medicinal slices of fresh Cordyceps sinensis obtained in Examples 1-4 and Comparative Examples 1-4 were taken and their overall appearance and microscopic appearance were observed. The results are as follows: Figures 1 to 32 As shown.

[0130] Conclusion: The freeze-dried Cordyceps sinensis slices obtained in Examples 1, 2, 3, and 4 have a neat and smooth overall appearance, and exhibit a three-dimensional network structure under microscopic observation (see...). Figures 1 to 16 This improves the physical strength of freeze-dried medicinal slices, making them less prone to breakage and allowing them to quickly absorb water and disperse upon contact, thus preventing them from adhering to the inner wall of the mouth. In contrast, the freeze-dried medicinal slices of fresh Cordyceps obtained in Comparative Examples 1, 2, 3, and 4 showed protrusions on their surface, resulting in a poor overall appearance and a two-dimensional sheet-like structure under microscopic examination (see...). Figures 17-32 This can cause problems such as easy adhesion to the inner wall of the mouth. This shows that neither wet ball milling alone nor gradient cooling pre-freezing alone can produce freeze-dried cakes with high physical strength, not easy to break, able to quickly absorb water and disintegrate after contact with water, and not easy to adhere to the inner wall of the mouth. However, the present invention prepares freeze-dried direct-drinking tablets by combining wet ball milling and gradient cooling pre-freezing, which can produce freeze-dried direct-drinking tablets with a neat and flat overall appearance, a three-dimensional network structure in microscopic appearance, high physical strength, not easy to break, able to quickly absorb water and disintegrate after contact with water, and not easy to adhere to the inner wall of the mouth.

[0131] Example 9: Sensory Evaluation

[0132] Twelve sensory evaluators were selected to conduct sensory evaluations on the appearance, aroma, and taste of the freeze-dried Cordyceps sinensis slices obtained in Examples 1-4 and Comparative Examples 1-4. The evaluation results of each evaluator were compiled and summarized, and the results are shown in Table 4.

[0133] Table 4: Sensory Evaluation Results

[0134]

[0135]

[0136] Conclusion: Compared with the freeze-dried medicinal slices obtained in Comparative Examples 1-4, the freeze-dried medicinal slices obtained in Examples 1-4 of this invention can retain the flavor of fresh medicinal materials very well. Moreover, they have a sponge-like structure, a large specific surface area, are easily dissolved through the oral mucosa, do not adhere to the oral cavity, and have no grainy feel.

[0137] The method of this invention has been described through preferred embodiments. Those skilled in the art will readily be able to modify or appropriately alter and combine the methods and applications described herein within the scope, spirit, and context of this invention to implement and apply the technology of this invention. Those skilled in the art can refer to the content herein to appropriately improve process parameters. It should be particularly noted that all similar substitutions and modifications are obvious to those skilled in the art and are considered to be included within the scope of this invention.

Claims

1. A method of making a composition comprising: Take the medicinal materials, add water, homogenize and pulverize them, the weight percentage of the medicinal materials in the total weight of water and medicinal materials is 7wt%~30wt%; wet ball milling, the particle size D90 of the medicinal material powder obtained after wet ball milling is ≤45μm; freeze-dry to obtain a composition, the composition is a direct-drinking medicinal slice, the freeze-drying includes pre-freezing, sublimation drying and desorption drying, the pre-freezing is carried out by gradient cooling; the medicinal materials are Cordyceps sinensis; and / or the medicinal materials are dried Cordyceps sinensis or fresh Cordyceps sinensis; wherein, the parameters of the pre-freezing are: Pre-freezing stage 1: Adjust the temperature to -5℃ within 30 minutes and maintain this temperature for 120 minutes, with a pressure of 0.09MPa~0.11MPa; Second stage of pre-freezing: Within 30 minutes, adjust the temperature to -20℃ and maintain this temperature for 120 minutes, with a pressure of 0.09MPa~0.11MPa; and The third stage of pre-freezing: Within 20-40 minutes, adjust the temperature to -40℃ and maintain this temperature for 120 minutes, with a pressure of 0.09MPa~0.11MPa; The parameters for the sublimation drying are: adjusting the temperature to -5°C within 60 minutes and maintaining this temperature for 1500 minutes, with a pressure of 13 Pa. The parameters for the analytical drying process are as follows: the temperature is adjusted to 25°C within 30 minutes and maintained at this temperature for 360 minutes, with a pressure of 13 Pa.

2. According to the method of claim 1, the operation steps of the wet ball milling are as follows: take ball milling beads with a particle size of 0.1 mm to 5 mm and ball mill them with the homogenized slurry after homogenization and crushing, the weight of the ball milling beads is 1 to 5 times the weight of the homogenized slurry, and the ball milling time is 30 min to 90 min.

3. A composition prepared by the method according to any one of claims 1-2.

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