Preparation method of traditional Chinese medicine decoction pieces

Through physical wall-breaking and assisted enzymatic solution and vacuum freeze-drying technology, combined with red date powder and wolfberry powder, the problem of underutilization of active substances in Dendrobium decoction tablets is solved, and the efficient extraction of Dendrobium polysaccharide and Dendrobium alkali and the solubleness of the decoction tablets is achieved.

CN120420385APending Publication Date: 2025-08-05SICHUAN KANGQUANTANG TRADITIONAL CHINESE MEDICINE PIECES
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Patent Information

Application Number
CN202510575913.4
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2025-05-06
Publication Date
2025-08-05

AI Technical Summary

Technical Problem

In the prior art, the nutrients of Dendrobium decoction tablets are difficult to efficiently utilize. Sliced soaking causes the residues of active substances such as polysaccharides and Dendrobium alkali in Dendrobium cells to be not fully released in the decoction tablets.

Method used

The physical wall-breaking assisted enzymatic solution is used to destroy the Dendrobium cell wall structure through laccase, cellulase and/or pectin enzyme. Combined with vacuum freeze-drying technology, Dendrobium powder is prepared and then mixed with red date powder and wolfberry powder to press the tablet to achieve efficient utilization of active ingredients.

Benefits of technology

Fully release active substances such as polysaccharides and dendrobium alkali in Dendrobium cells, reduce the use of binders, and prepare them into easily dissolved Chinese herbal medicines, suitable for a variety of people.

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Abstract

The invention discloses a preparation method of traditional Chinese medicine decoction pieces, and relates to the technical field of traditional Chinese medicine processing. Comprising the following steps: crushing dendrobium stems to prepare dendrobium coarse powder; soaking the dendrobe coarse powder in deionized water to prepare a mixed solution, adjusting the pH value of the mixed solution, and adding an enzymolysis agent in batches to obtain an enzymolysis mixed solution; carrying out reduced-pressure suction filtration on the enzymolysis mixed liquid, collecting filtrate and residues, and carrying out reduced-pressure concentration on the obtained filtrate to obtain an extract concentrated solution; performing vacuum freeze drying on the extract concentrated solution to obtain dendrobium nobile powder; and adding red date powder and Chinese wolfberry fruit powder into the dendrobium nobile stem powder to prepare the dendrobium nobile stem decoction pieces. The enzymolysis agent comprises laccase, cellulase and / or pectinase. Dendrobium nobile powder prepared by a physical wall-breaking assisted enzymolysis method is mixed with the red date powder and the Chinese wolfberry fruit powder, and then the mixture can be directly tableted and formed without additionally adding a binder.
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Description

Technical Field

[0001] The present invention relates to the technical field of Chinese medicinal slices, and in particular to a preparation method of Chinese medicinal slices. Background Art

[0002] Dendrobium refers to the cultivated varieties of Dendrobium nobile, Dendrobium candidum, Dendrobium chrysotoxum, and Dendrobium tasselata, as well as the fresh or dried stems of related species of the Orchidaceae family. Dendrobium is a traditional Chinese medicinal herb with rich medicinal properties, containing a variety of active ingredients. Dendrobium polysaccharides are the main active ingredient in Dendrobium, exhibiting multiple biological activities, including immunomodulatory, anti-tumor, anti-inflammatory, antioxidant, hypoglycemic, and lipid-lowering properties. Dendrobium alkaloids, a type of alkaloid found in Dendrobium, have anti-tumor, hypoglycemic, and anti-aging effects. Phenanthrene compounds, including chrysotoxum and eriocin, exhibit anti-tumor activity, particularly against lung cancer, ovarian cancer, and leukemia cells. Dendrobium contains 18 amino acids, seven of which are essential for the human body, and possesses antioxidant, anti-aging, liver-protecting, and lung-moisturizing properties. Furthermore, Dendrobium is rich in trace elements such as calcium, iron, zinc, selenium, and magnesium, which help regulate metabolism and enhance immunity.

[0003] Prior art CN108310228A discloses a dendrobium decoction slice and its preparation method. The slice is made from the following ingredients: dendrobium, sucralose, lemon juice, and yellow vinegar. The dendrobium decoction slice of the invention is ready to drink, has a delicate taste, a mellow color, and stable medicinal efficacy. However, the dendrobium decoction slice of the invention is only sliced and brewed, which also results in residual nutrients in the slice that cannot be efficiently utilized. Summary of the Invention

[0004] The purpose of the present invention is to provide a preparation method of Chinese herbal medicine slices, which destroys the cell wall structure of Dendrobium officinale by physical wall breaking assisted enzymatic hydrolysis, fully releases polysaccharides, dendrobine, pectin and other active substances in the Dendrobium cells, and prepares the Chinese herbal medicine slices into compressed tablets without using an external binder, thereby achieving efficient utilization of the effective ingredients of Dendrobium.

[0005] A method for preparing Chinese medicinal slices comprises the following steps:

[0006] Step 1: Grind the stems of Dendrobium officinale to prepare coarse Dendrobium officinale powder;

[0007] Step 2: Soaking the above-mentioned coarse powder of Dendrobium officinale in deionized water to prepare a mixed solution, adjusting the pH of the mixed solution to 4.5-6.0, adding an enzymatic hydrolyzing agent in batches, and fully reacting at a reaction temperature of 45° C.-70° C. for 7-10 hours to obtain an enzymatic hydrolysis mixed solution;

[0008] Step 3: Filter the enzymatic hydrolysis mixture under reduced pressure, collect the filtrate and residue, and repeat step 2 with the residue to continue enzymatic hydrolysis;

[0009] Step 4: Concentrating the filtrate obtained in step 3 under reduced pressure to obtain an extract concentrate;

[0010] Step 5: vacuum freeze-drying the extract concentrate to obtain dendrobium powder;

[0011] Step 6: Add red date powder and wolfberry powder to the above-mentioned dendrobium powder, press into slices, and make dendrobium decoction slices.

[0012] The mass ratio of the dendrobium powder to the enzymatic hydrolyzing agent is 100:1-5, and the enzymatic hydrolyzing agent includes laccase, cellulase and / or pectinase.

[0013] The present invention uses laccase, cellulase and / or pectinase as enzymolysis agents to enzymolyze coarse dendrobium powder, destroys the dendrobium cell wall structure by the enzymolysis agents, fully releases active ingredients such as dendrobium polysaccharides and dendrobium alkaloids in the dendrobium cells, collects the active ingredients by decompression filtration and decompression concentration, and prepares the collected active ingredients into dendrobium powder by freeze drying. The powder is then mixed with red date powder and wolfberry powder and pressed into tablets to obtain dendrobium Chinese medicinal slices. During the preparation process, it was found that by adjusting the components, component contents, order of addition of the enzymolysis agents, and enzymolysis time of the enzymolysis agents, not only the extraction amount of dendrobium polysaccharides and dendrobium alkaloids can be affected, but also whether an additional binder needs to be added when the dendrobium mixed powder is pressed into tablets can be affected.

[0014] Furthermore, the enzymatic agent includes pectinase and laccase, the mass ratio of the pectinase to the laccase is 1 to 2:1, and the method for adding the enzymatic agent is: adjusting the pH of the mixture to 4.5 to 5.5, adding pectinase, raising the temperature to 45 to 55°C, and reacting for 2 to 3 hours; adjusting the pH of the mixed solution to 5.0 to 6.0, continuing to add laccase, raising the temperature to 60 to 70°C, and reacting for 5 to 7 hours; after the reaction is completed, raising the temperature to 75 to 80°C.

[0015] During the preparation process, it was found that the use of pectinase and laccase resulted in higher extraction amounts of dendrobium polysaccharides and dendrobium alkaloids. When pectinase and laccase were added in batches, the benefits of the dendrobium polysaccharides, dendrobium alkaloids, and dendrobium powder obtained after enzymolysis were significantly improved compared to when the two enzymes were added simultaneously. The applicant believes that the optimal pH and temperature suitable for the two enzymes, pectinase and laccase, are different. Adding them simultaneously not only fails to achieve the normal performance of the two enzyme activities, but may also result in the activity of one of the enzymes being inhibited. In addition, as the enzymolysis time increases, the extraction amount of dendrobium polysaccharides and dendrobium alkaloids does not continue to increase, and the obtained dendrobium powder, when compressed with red date powder and wolfberry powder, requires the addition of more binding agents. In the present invention, the binding agent is selected as a cellulose binding agent.

[0016] In order to fully extract the active substances in the dendrobium, while reducing the amount of binder used or not using a binder, the inventor adjusted the method: reducing the amount of pectinase added. Under the premise of unchanged reaction time, the extracted amount of dendrobium polysaccharides and dendrobium alkaloids obtained and the income of dendrobium powder will be reduced. Considering the reason, it may be that reducing the amount of pectinase added causes the density of pectinase in the mixed solution to decrease, resulting in the inability to complete the effective destruction of the cell wall within the reaction time, so that the active ingredients cannot be fully released. If the amount of pectinase added is kept unchanged and the reaction time is gradually shortened, it is found that the extracted amount of dendrobium polysaccharides and dendrobium alkaloids obtained will not be significantly reduced, but the binder required during tableting will be significantly reduced, and the income of dendrobium powder will be significantly improved.

[0017] Determination of the extracted active ingredients revealed that pectinase, when present in sufficient amounts, can break down pectin into small molecules. As the pectinase content gradually decreases, the pectin content in the extract gradually increases. Therefore, as the amount of pectin extracted increases, the amount of binder required for tableting decreases significantly. This is likely because pectin forms new cross-linked structures with the extracted dendrobium polysaccharides, dendrobium alkaloids, and certain components of red date and wolfberry powders, replacing the binder.

[0018] Furthermore, the enzymatic agent includes cellulase and laccase, and the mass ratio of the cellulase to laccase is 1:3.3~5.0; the method for adding the enzymatic agent is: adjusting the pH of the mixture to 5.0~6.0, adding cellulase, raising the temperature to 45~60°C, and reacting for 5~7h; keeping the pH of the mixed solution unchanged, continue to add laccase, raise the temperature to 60~70°C, and react for 3~5h; after the reaction is completed, adjust the pH of the mixed solution to 7.0~8.0.

[0019] With cellulase replacing pectinase, and combining with laccase to carry out enzymatic hydrolysis and wall breaking of coarse powder of dendrobium, it is found that adding cellulase first and then adding laccase, compared with the simultaneous addition of two enzymes, can significantly improve the content of dendrobium polysaccharide and pectin in the extract, and when pressed into tablets, no binding agent is needed. However, the content of dendrobium alkaloids is always lower than that using pectinase-laccase wall breaking, and the income of dendrobium powder is slightly lower than that of pectinase-laccase wall breaking. The inventor guesses that it may be that new active ingredients are formed in the enzymolysis solution after the action of cellulase and laccase, causing the partial decomposition of dendrobium alkaloids.

[0020] Furthermore, the method for processing the dry stems of Dendrobium is as follows: cleaning the dry stems of Dendrobium, drying the surface moisture, cutting into 0.4cm-0.8cm segments, and crushing to a particle size of 1-100μm to obtain coarse Dendrobium powder.

[0021] Furthermore, in step 2, the dendrobium crude powder is poured into deionized water at 25-35° C. according to a solid-liquid ratio of 1:5-10, stirred to form a mixed solution, and stirred continuously for 1-3 hours to fully soak the dendrobium crude powder.

[0022] Furthermore, the method of vacuum concentration in step 4 is: vacuum concentration of the filtrate collected in step 3 at a temperature of 40-45° C. and a pressure of 7-12 kPa, until the volume becomes 1 / 5-1 / 4 of the original volume.

[0023] Furthermore, in step 5, the vacuum freeze-drying step includes the following:

[0024] In the pre-freezing stage, the temperature is -40 to -50°C for 2 to 5 hours to quickly freeze the dendrobium powder;

[0025] Primary drying: temperature -15~-30℃, vacuum degree 10~50Pa, time 15~20h, remove surface moisture;

[0026] Secondary drying: gradually increase the temperature to 20-40°C, vacuum degree 1-10 Pa, time 4-8h, to remove crystal water.

[0027] Vacuum freeze-drying can maximize the retention of active ingredients in Dendrobium, ensuring its medicinal efficacy and nutritional value; at the same time, it can effectively retain the natural color and flavor of Dendrobium, and improve the sensory quality of the product.

[0028] Furthermore, in step six, by weight, 60 to 80 parts of dendrobium powder, 8 to 10 parts of red date powder, and 3 to 5 parts of wolfberry powder are used; the preparation method of the red date powder comprises: grinding and peeling dried red dates, and then crushing them into red date powder with a particle size of 1 to 20 μm; the particle size of the wolfberry powder is 1 to 20 μm.

[0029] Furthermore, in step six, the step of pressing into tablets includes: mixing dendrobium powder, red date powder and wolfberry powder in a proportion to form a mixed powder, and using a tablet press to press the mixed powder into tablets under a pressure of 10 to 20 kN, wherein the specification of the tablets is 0.5 to 1.0 g / tablet.

[0030] By making Dendrobium Chinese herbal medicine slices into tablets of specific quality specifications, they can be taken in fixed quantities as needed and are convenient to carry.

[0031] Cellulase (β-1,4-glucan-4-glucanohydrolase) is a general term for a group of enzymes that degrade cellulose to produce glucose. It is not a monomeric enzyme, but a multi-component enzyme system that works synergistically. It is a complex enzyme mainly composed of exo-β-glucanase, endo-β-glucanase and β-glucosidase, as well as highly active xylanase.

[0032] Laccase is a polyphenol oxidase containing four copper ions (ρ-diphenol oxidase, EC 1.10.3.2), which belongs to the copper blue oxidase and exists in the form of a monomeric glycoprotein.

[0033] Pectinase refers to enzymes that break down pectin, the main component of plants, including pectinesterase and polygalacturonase.

[0034] The beneficial effects of the present invention are:

[0035] 1. The present invention destroys the cell wall structure of Dendrobium officinale through a physical wall-breaking assisted enzymatic hydrolysis method, fully releasing multiple active substances such as polysaccharides, dendrobium alkaloids, and pectin in the Dendrobium cells, thereby achieving effective utilization of the effective ingredients of Dendrobium; and when the weight ratio of Dendrobium powder, red date powder, and wolfberry powder is 60-80:8-10:3-5, when the pectin content in the prepared Dendrobium powder is between 5.2% and 5.7%, the mixed powder can be directly compressed into tablets without the need for additional binding agents, has moderate hardness, and is easily soluble in water.

[0036] 2. Red dates and wolfberries are added to the dendrobium powder of the present invention to form a new active cross-linked structure with the extracted active substances, which can replace the binder required for tableting; at the same time, it effectively neutralizes the coldness of dendrobium, can be taken with warm water, can be quickly dissolved, and increases the number of people who are applicable to the dendrobium powder slices. DETAILED DESCRIPTION

[0037] The technical solution of the present invention is described clearly and completely below. Obviously, the embodiments described here are only a part of the present invention, rather than all the embodiments.

[0038] Material:

[0039] Dried stems of Dendrobium officinale, produced in Yunnan, moisture ≤10%; dried red dates, moisture ≤8%, produced in Xinjiang; dried wolfberry fruit, moisture ≤5%, produced in Ningxia; enzymatic hydrolyzers are commercially available.

[0040] Example 1

[0041] A method for preparing Chinese medicinal slices comprises the following steps:

[0042] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.4 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0043] Step 2: Soak the Dendrobium powder in 500 ml of 25°C deionized water and stir for 1 hour, then adjust the pH to 4.5 with acetic acid-sodium acetate buffer solution, add 1.0 g of pectinase, and raise the temperature to 45°C for pre-reaction for 3 hours; adjust the pH to 5.0, add 1.0 g of laccase, and react for 5 hours. After thorough mixing, the reaction temperature is 60°C, and the reaction is continuously stirred; after the reaction is complete, the temperature is raised to 75°C to quench the enzymatic reaction.

[0044] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0045] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 40°C and a pressure of 7 kPa, to obtain the target extract;

[0046] Step 5: pre-freeze the target extract at -50°C; sublimate and dry at -25°C under a vacuum of 25Pa; and decompose and dry by gradually increasing the temperature to 30°C under a vacuum of 7Pa to obtain 64.6g of Dendrobium powder.

[0047] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0048] Example 2

[0049] A method for preparing Chinese medicinal slices comprises the following steps:

[0050] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.8 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0051] Step 2: Soak the Dendrobium powder in 800 ml of 35°C deionized water and stir for 1.5 hours, then adjust the pH to 5.5 with acetic acid-sodium acetate buffer solution, add 3.0 g of pectinase, raise the temperature to 55°C for pre-reaction for 2.5 hours; add 2.0 g of laccase and react for 6 hours. After thorough mixing, the reaction temperature is 70°C and the reaction is continuously stirred; after the reaction is complete, the temperature is raised to 80°C to quench the enzymatic reaction.

[0052] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0053] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 4 of the original volume, at a temperature of 45°C and a pressure of 10 kPa, to obtain the target extract;

[0054] Step 5: Prefreeze the target extract at -40°C; dry it once at -30°C and a vacuum of 10Pa; and dry it twice, gradually raising the temperature to 20°C and a vacuum of 10Pa to obtain 66.8g of Dendrobium powder.

[0055] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0056] Example 3

[0057] A method for preparing Chinese medicinal slices comprises the following steps:

[0058] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.6 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0059] Step 2: Soak the Dendrobium powder in 1000 ml of 35°C deionized water and stir for 3 hours, then adjust the pH to 5.0 with acetic acid-sodium acetate buffer solution, add 2.0 g of pectinase, raise the temperature to 45°C for pre-reaction for 2 hours; adjust the pH to 6.0, add 1.0 g of laccase, react for 5 hours, mix thoroughly, and set the reaction temperature to 70°C with continuous stirring; after the reaction is complete, raise the temperature to 80°C to quench the enzymatic reaction.

[0060] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0061] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 42°C and a pressure of 12 kPa, to obtain the target extract;

[0062] Step 5: pre-freeze the target extract at -45°C; sublimate and dry at -15°C under a vacuum of 50Pa; and decompose and dry by gradually increasing the temperature to 40°C and a vacuum of 9Pa to obtain 67.7g of Dendrobium powder.

[0063] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0064] Example 4

[0065] A method for preparing Chinese medicinal slices comprises the following steps:

[0066] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.6 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0067] Step 2: Soak the Dendrobium powder in 1000 ml of 35°C deionized water and stir for 2.5 hours. Then, adjust the pH to 5.2 with acetic acid-sodium acetate buffer solution, add 2.1 g of pectinase, raise the temperature to 45°C for pre-reaction for 2.3 hours; adjust the pH to 6.0, add 0.9 g of laccase, and react for 5 hours. After thorough mixing, the reaction temperature is 70°C, and the reaction is continuously stirred; after the reaction is complete, raise the temperature to 80°C to quench the enzymatic reaction.

[0068] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0069] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 42°C and a pressure of 12 kPa, to obtain the target extract;

[0070] Step 5: pre-freeze the target extract at -45°C; sublimate and dry at -15°C under a vacuum of 50 Pa; and decompose and dry by gradually increasing the temperature to 40°C under a vacuum of 9 Pa to obtain 67.1 g of Dendrobium powder.

[0071] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0072] Comparative Example 1

[0073] A method for preparing Chinese medicinal slices comprises the following steps:

[0074] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.4 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0075] Step 2: Soak the Dendrobium powder in 500 ml of 25°C deionized water and stir for 1 hour, then adjust the pH to 5.0 with acetic acid-sodium acetate buffer solution, add 1.0 g pectinase and 1.0 g laccase, and react for 7 hours. After thorough mixing, the reaction temperature is 55-60°C and stirring is continued; after the reaction is complete, the temperature is raised to 75°C to quench the enzymatic hydrolysis reaction.

[0076] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0077] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 40°C and a pressure of 7 kPa, to obtain the target extract;

[0078] Step 5: pre-freeze the target extract at -50°C; sublimate and dry at -25°C and a vacuum degree of 25Pa; and decompose and dry by gradually increasing the temperature to 30°C and a vacuum degree of 7Pa to obtain 55.3g of Dendrobium powder.

[0079] Comparative Example 2

[0080] A method for preparing Chinese medicinal slices comprises the following steps:

[0081] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.8 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0082] Step 2: Soak the Dendrobium powder in 800 ml of 35°C deionized water and stir for 1.5 hours. Then, adjust the pH to 5.5 with acetic acid-sodium acetate buffer solution, add 3.0 g of pectinase, raise the temperature to 55°C for pre-reaction for 5 hours; add 2.0 g of laccase and react for 6 hours. After thorough mixing, the reaction temperature is 70°C and the reaction is continuously stirred; after the reaction is complete, raise the temperature to 80°C to quench the enzymatic reaction.

[0083] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0084] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 4 of the original volume, at a temperature of 45°C and a pressure of 10 kPa, to obtain the target extract;

[0085] Step 5: pre-freeze the target extract at -40°C; perform primary drying at -30°C and a vacuum degree of 10Pa; perform secondary drying by gradually increasing the temperature to 20°C and a vacuum degree of 10Pa; and obtain 62.8 g of Dendrobium powder.

[0086] Comparative Example 3

[0087] A method for preparing Chinese medicinal slices comprises the following steps:

[0088] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.6 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0089] Step 2: Soak the Dendrobium powder in 1000 ml of 35°C deionized water and stir for 3 hours, then adjust the pH to 5.0 with acetic acid-sodium acetate buffer solution, add 2.0 g of pectinase, raise the temperature to 45°C for pre-reaction for 4 hours; adjust the pH to 6.0, add 1.0 g of laccase, react for 5 hours, mix thoroughly, and set the reaction temperature to 70°C with continuous stirring; after the reaction is complete, raise the temperature to 80°C to quench the enzymatic reaction.

[0090] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0091] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 42°C and a pressure of 12 kPa, to obtain the target extract;

[0092] Step 5: pre-freeze the target extract at -45°C; sublimate and dry at -15°C and a vacuum degree of 50Pa; and decompose and dry by gradually increasing the temperature to 40°C and a vacuum degree of 9Pa to obtain 64.5g of Dendrobium powder.

[0093] Example 5

[0094] A method for preparing Chinese medicinal slices comprises the following steps:

[0095] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.5 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0096] Step 2: Soak the Dendrobium powder in 500 ml of 25°C deionized water and stir for 1 hour, then adjust the pH to 5.0 with acetic acid-sodium acetate buffer solution, add 0.47 g of cellulase, raise the temperature to 45°C and pre-react for 5 hours; then add 1.53 g of laccase and react for 3 hours. After thorough mixing, the reaction temperature is 62°C and the reaction is continuously stirred; adjust the pH of the mixed solution to 7.0 to quench the enzymatic reaction.

[0097] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0098] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 40°C and a pressure of 7 kPa, to obtain the target extract;

[0099] Step 5: pre-freeze the target extract at -50°C; sublimate and dry at -25°C and a vacuum of 25Pa; and decompose and dry by gradually increasing the temperature to 30°C and a vacuum of 7Pa to obtain 61.6g of Dendrobium powder.

[0100] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0101] Example 6

[0102] A method for preparing Chinese medicinal slices comprises the following steps:

[0103] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.7 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0104] Step 2: Soak the Dendrobium powder in 800 ml of 35°C deionized water and stir for 1.5 hours. Then, adjust the pH to 5.5 with acetic acid-sodium acetate buffer solution, add 1.0 g of cellulase, raise the temperature to 55°C and pre-react for 7 hours; then add 4.0 g of laccase and react for 4 hours. After thorough mixing, the reaction temperature is 68°C and the reaction is continuously stirred; adjust the pH of the mixed solution to 8.0 to quench the enzymatic reaction.

[0105] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0106] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 4 of the original volume, at a temperature of 45°C and a pressure of 10 kPa, to obtain the target extract;

[0107] Step 5: Prefreeze the target extract at -40°C; dry it once at -30°C and a vacuum of 10Pa; and dry it twice, gradually raising the temperature to 20°C and a vacuum of 10Pa to obtain 63.2g of Dendrobium powder.

[0108] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0109] Example 7

[0110] A method for preparing Chinese medicinal slices comprises the following steps:

[0111] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.6 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0112] Step 2: Soak the Dendrobium powder in 1000 ml of 35°C deionized water and stir for 6 hours, then adjust the pH to 6.0 with acetic acid-sodium acetate buffer solution, add 0.5 g of cellulase, raise the temperature to 60°C and pre-react for 7 hours; then add 2.5 g of laccase and react for 5 hours. After thorough mixing, the reaction temperature is 70°C and the reaction is continuously stirred; adjust the pH of the mixed solution to 7.5 to quench the enzymatic reaction.

[0113] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0114] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 42°C and a pressure of 12 kPa, to obtain the target extract;

[0115] Step 5: pre-freeze the target extract at -45°C; sublimate and dry at -15°C under a vacuum of 50Pa; and decompose and dry by gradually increasing the temperature to 40°C under a vacuum of 9Pa to obtain 62.5g of Dendrobium powder.

[0116] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0117] Example 8

[0118] A method for preparing Chinese medicinal slices comprises the following steps:

[0119] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.7 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0120] Step 2: Soak the Dendrobium powder in 800 ml of 35°C deionized water and stir for 6 hours, then adjust the pH to 6.0 with acetic acid-sodium acetate buffer solution, add 0.58 g of cellulase, raise the temperature to 60°C and pre-react for 7 hours; then add 2.42 g of laccase and react for 5 hours. After thorough mixing, the reaction temperature is 65°C and the reaction is continuously stirred; adjust the pH of the mixed solution to 8.0 to quench the enzymatic reaction.

[0121] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0122] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 42°C and a pressure of 12 kPa, to obtain the target extract;

[0123] Step 5: pre-freeze the target extract at -45°C; sublimate and dry at -15°C under a vacuum of 50Pa; and decompose and dry by gradually increasing the temperature to 40°C under a vacuum of 9Pa to obtain 63.3g of Dendrobium powder.

[0124] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0125] Comparative Example 4

[0126] A method for preparing Chinese medicinal slices comprises the following steps:

[0127] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.4 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0128] Step 2: Soak the Dendrobium powder in 500 ml of 25°C deionized water and stir for 1 hour. Then, adjust the pH to 5.0 with acetic acid-sodium acetate buffer solution, add 0.47 g of cellulase, and then add 1.53 g of laccase to react for 3 hours. After thorough mixing, the reaction temperature is 50-60°C and the reaction is continuously stirred; adjust the pH of the mixed solution to 7.0 to quench the enzymatic hydrolysis reaction.

[0129] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0130] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 40°C and a pressure of 7 kPa, to obtain the target extract;

[0131] Step 5: pre-freeze the target extract at -50°C; sublimate and dry at -25°C under a vacuum of 25Pa; and decompose and dry by gradually increasing the temperature to 30°C under a vacuum of 7Pa to obtain 51.2g of Dendrobium powder.

[0132] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0133] Comparative Example 5

[0134] A method for preparing Chinese medicinal slices comprises the following steps:

[0135] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.6 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0136] Step 2: Soak the Dendrobium powder in 1000 ml of 35°C deionized water and stir for 3 hours, then adjust the pH to 5.0 with acetic acid-sodium acetate buffer solution, add 2.5 g of pectinase, raise the temperature to 45°C for pre-reaction for 2 hours; adjust the pH to 6.0, add 1.0 g of laccase, react for 5 hours, mix thoroughly, and set the reaction temperature to 70°C with continuous stirring; after the reaction is complete, raise the temperature to 80°C to quench the enzymatic reaction.

[0137] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0138] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 42°C and a pressure of 12 kPa, to obtain the target extract;

[0139] Step 5: pre-freeze the target extract at -45°C; sublimate and dry at -15°C under a vacuum of 50Pa; and decompose and dry by gradually increasing the temperature to 40°C and a vacuum of 9Pa to obtain 63.0g of Dendrobium powder.

[0140] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0141] Comparative Example 6

[0142] A method for preparing Chinese medicinal slices comprises the following steps:

[0143] Step 1: Cut 100 g of dry stems of Dendrobium officinale into 0.6 cm segments, and ultrafinely grind them to a particle size of 1 to 20 μm to obtain Dendrobium officinale powder;

[0144] Step 2: Soak the Dendrobium powder in 1000 ml of 35°C deionized water and stir for 3 hours, then adjust the pH to 5.0 with acetic acid-sodium acetate buffer solution, add 0.5 g of pectinase, raise the temperature to 45°C for pre-reaction for 2 hours; adjust the pH to 6.0, add 1.0 g of laccase, react for 5 hours, mix thoroughly, and set the reaction temperature to 70°C with continuous stirring; after the reaction is complete, raise the temperature to 80°C to quench the enzymatic reaction.

[0145] Step 3: Filter out the residue under reduced pressure using 5-20 μm filter paper and collect the filtrate;

[0146] Step 4: Concentrate the filtrate under reduced pressure until the volume of the filtrate becomes 1 / 5 of the original volume, at a temperature of 42°C and a pressure of 12 kPa, to obtain the target extract;

[0147] Step 5: pre-freeze the target extract at -45°C; sublimate and dry at -15°C under a vacuum of 50Pa; and decompose and dry by gradually increasing the temperature to 40°C and a vacuum of 9Pa to obtain 48.2g of Dendrobium powder.

[0148] Step 6: Add red date powder and wolfberry powder to the dendrobium powder obtained above, mix well and compress into tablets using a tablet press.

[0149] The contents of dendrobium polysaccharide, dendrobine and pectin in Examples 1-3 and Comparative Examples 4-6 were determined by high performance liquid chromatography on the obtained dendrobium powder. The results are shown in Table 1.

[0150] Table 1 Contents of polysaccharides, dendrobine and pectin in Examples 1-3 and Comparative Examples 4-6 and the quality of the obtained dendrobium powder

[0151] Pectinase reaction pH Pectinase reaction time Dendrobium polysaccharide content Dendrobium alkaloid content Pectin content Quality of Dendrobium powder obtained Example 1 4.5 3h 16.5% 11.2% 4.2% 64.6g Example 2 5.5 2.5h 16.2% 10.8% 4.9% 66.8g Example 3 5.0 2h 16.7% 10.3% 5.2% 67.7g Example 4 5.2 2.3 16.6% 10.7% 5.5% 67.1g Comparative Example 1 4.5 7h 12.1% 7.9% - 55.3g Comparative Example 2 5.5 5h 16.5% 10.2% - 62.8g Comparative Example 3 5.0 4h 16.9% 10.6% - 64.5g

[0152] Note: “-” in Table 1 means the pectin content was not measured.

[0153] As shown in Table 1, in Comparative Example 1, pectinase and laccase were added to the mixed solution at the same time for enzymolysis. Compared with Examples 1 to 4, the measured dendrobium polysaccharides, dendrobine and the quality of the obtained dendrobium powder were significantly reduced, indicating that the present invention adds pectinase and laccase to the mixed solution in stages to enzymolyze the stems of Dendrobium officinale, which can effectively increase the extraction amount of dendrobium polysaccharides and dendrobine and the profit of dendrobium powder.

[0154] In Comparative Examples 1-3, the action time of pectinase was prolonged, and almost no pectin was detected in the collected Dendrobium powder, indicating that the pectin was completely decomposed; and the profit of the Dendrobium powder did not increase with the increase in the action time of pectinase.

[0155] In Example 3, when the pectinase reaction pH = 5.0, the pectinase reaction time is 2h, at this time the pectin content in the extract is 5.2%, and the maximum yield of Dendrobium powder is 67.7g; in Example 4, when the pectinase reaction pH = 5.2, the pectinase reaction time is 2.3h, at this time the pectin content in the extract is 5.5% and the maximum yield of Dendrobium powder is 67.1g.

[0156] In Examples 5-7 and Comparative Example 4, cellulase and laccase were used to enzymatically hydrolyze the stems of Dendrobium officinale, and the contents of dendrobium polysaccharides, dendrobine and pectin in the Dendrobium powder were determined by high performance liquid chromatography. The results are shown in Table 2.

[0157] Table 2 Contents of Dendrobium polysaccharides, dendrobine and pectin

[0158] Cellulase:Laccase Whether to join in batches Dendrobium polysaccharide content Dendrobium alkaloid content Pectin content Quality of Dendrobium powder obtained Example 5 1:3.3 yes 15.7% 9.2% 6.5% 61.6g Example 6 1:4 yes 16.9% 8.4% 6.9% 63.2g Example 7 1:5 yes 16.1% 8.7% 5.7% 62.5g Example 8 1:4.4 yes 16.8% 8.7% 6.1% 63.3g Comparative Example 4 1:3.3 no 13.1% 6.8% 4.7% 51.2g

[0159] As shown in Table 2, in Examples 5-8, the enzymolysis agent was added in batches. Compared with the two enzymolysis agents of Comparative Example 4, which were added simultaneously, the dendrobium polysaccharide, dendrobium alkaloids and pectin content and the dendrobium powder income were significantly higher, indicating that the enzymolysis agent batch addition method of the present invention can significantly improve the dendrobium polysaccharide, dendrobium alkaloids and pectin content and the dendrobium powder income. A higher pectin content can also be obtained than when using pectinase and laccase as enzymolysis agents. However, compared with using pectinase and laccase as enzymolysis agents in Examples 1-4, the dendrobium powder income obtained is relatively low.

[0160] The dendrobium powder obtained in Examples 1-8 was mixed with red date powder and wolfberry powder, respectively, and then pressed into Chinese herbal medicine slices. The molding conditions are shown in Table 3.

[0161] Table 3 Forming of the Dendrobium powder obtained in Examples 1-8, mixed with red date powder and wolfberry powder to form Chinese herbal medicine slices

[0162] Weight ratio of dendrobium, red dates and wolfberry Pectin content in Dendrobium powder Quality of Dendrobium powder obtained Forming state of the medicinal pieces Example 1 60~80:8~10:3~5 4.2% 64.6g - Example 2 60~80:8~10:3~5 4.9% 66.8g - Example 3 60~80:8~10:3~5 5.2% 67.7g + Example 4 60~80:8~10:3~5 5.5% 67.1g + Example 5 60~80:8~10:3~5 6.5% 61.6g ++ Example 6 60~80:8~10:3~5 6.9% 63.2g ++ Example 7 60~80:8~10:3~5 5.7% 62.5g + Example 8 60~80:8~10:3~5 6.1% 63.3g ++

[0163] Note: In Table 3, “-” indicates that the material cannot be formed or is easily disintegrated after forming; “+” indicates that the material can be formed with appropriate hardness and is easily soluble in water; and “++” indicates that the material can be formed with excessive hardness and is not easily soluble in water.

[0164] As shown in Table 3, when the weight ratio of dendrobium powder, red date powder, and wolfberry powder is 60-80:8-10:3-5, when the pectin content in the dendrobium powder is between 5.2% and 5.7%, the mixed powder can be formed and has a moderate hardness and is easily soluble in water; when the pectin content in the dendrobium powder is less than 4.9%, the mixed powder cannot be formed or easily collapses after forming; when the pectin content in the dendrobium powder is not less than 6.1%, the mixed powder can be formed and has too high a hardness and is not easily soluble in water. Therefore, the dendrobium powder prepared by the methods of Examples 3, 4, and 7, after being mixed with the dendrobium powder, red date powder, and wolfberry powder in a weight ratio of 60-80:8-10:3-5, can be directly compressed into tablets without adding an external binder, and is easily soluble in water.

[0165] For the dendrobium powder prepared in Example 1 and Example 2, the weight proportions of dendrobium powder, red date powder, and wolfberry powder were adjusted. It was found that the dendrobium powder prepared in Example 2, when the weight proportions of dendrobium powder, red date powder, and wolfberry powder were 60-80:15-20:3-5, the mixed powder could be pressed into shape and was easily soluble in water; whereas the dendrobium powder prepared in Example 1 required additional addition of a binder to be formed.

[0166] Exploring the relationship between the amount of pectinase added and the molding of Chinese herbal medicine slices: In Comparative Examples 5 and 6, after adding excess or insufficient pectinase, the obtained dendrobium powder was mixed with red date powder and wolfberry powder to make Chinese herbal medicine slices, as shown in Table 4.

[0167] Table 4 Exploration of the relationship between the amount of pectinase added and the molding of Chinese herbal medicine pieces

[0168] Amount of pectinase added Laccase addition amount Dendrobium powder quality Pectin content in Dendrobium powder Mixed powder molding state Example 3 2g 1g 67.7g 5.2% + Comparative Example 5 2.5g 1g 63.0g 4.1% - Comparative Example 6 0.5g 1g 48.2g 3.7% -

[0169] Note: In Table 4, “-” indicates that the product cannot be formed or easily collapses after forming, and “+” indicates that the product can be formed with appropriate hardness and is easily soluble in water.

[0170] As can be seen from Table 4, in Comparative Example 5, the amount of pectinase added was 2.5 g, and the amount of laccase added was 1.0 g, which was greater than the mass ratio of pectinase to laccase of 1 to 2: 1 in the present invention. The content of the obtained dendrobium powder was significantly reduced compared with Example 3, and the pectin content in the obtained dendrobium powder was significantly lower than that in Example 3. The mixed powder could not be formed or easily collapsed after forming. In Comparative Example 6, the amount of pectinase added was 0.5 g, and the amount of laccase added was 1.0 g, which was less than the mass ratio of pectinase to laccase of 1 to 2: 1 in the present invention. The content of the obtained dendrobium powder was significantly reduced compared with Example 3, and the pectin content in the obtained dendrobium powder was significantly lower than that in Example 3. The mixed powder could not be formed or easily collapsed after forming. In the present invention, when the mass ratio of pectinase to laccase is 1-2:1, the pectin content in the obtained dendrobium powder can be controlled by shortening the enzymatic hydrolysis time of the pectinase on the dendrobium officinale. When the dendrobium powder, red date powder and wolfberry powder are mixed in a weight ratio of 60-80:8-10:3-5, the mixture can be directly pressed into tablets without adding an external binder to prepare Chinese medicinal slices, and the Chinese medicinal slices are easily soluble in water.

Claims

1. A method for preparing Chinese herbal medicine slices, characterized in that: The following steps are involved: Step 1: Grind the stems of Dendrobium officinale to prepare coarse Dendrobium officinale powder; Step 2: Soaking the above-mentioned coarse powder of Dendrobium officinale in deionized water to prepare a mixed solution, adjusting the pH of the mixed solution to 4.5-6.0, adding an enzymatic hydrolyzing agent in batches, and fully reacting at a reaction temperature of 45° C.-70° C. for 7-10 hours to obtain an enzymatic hydrolysis mixed solution; Step 3: Filter the enzymatic hydrolysis mixture under reduced pressure, collect the filtrate and residue, and repeat step 2 with the residue to continue enzymatic hydrolysis; Step 4: Concentrating the filtrate obtained in step 3 under reduced pressure to obtain an extract concentrate; Step 5: vacuum freeze-drying the extract concentrate to obtain dendrobium powder; Step 6: Add red date powder and wolfberry powder to the above-mentioned dendrobium powder, press into slices, and make dendrobium decoction slices. The mass ratio of the dendrobium coarse powder to the enzymatic hydrolyzing agent is 100:2-5, and the enzymatic hydrolyzing agent includes laccase, cellulase and / or pectinase.

2. The method for preparing Chinese medicinal pieces according to claim 1, wherein: The enzymatic agent includes pectinase and laccase, and the mass ratio of the pectinase to the laccase is 1 to 2:

1. The method for adding the enzymatic agent is as follows: adjusting the pH of the mixture to 4.5 to 5.5, adding pectinase, raising the temperature to 45 to 55° C., and reacting for 2 to 3 hours; adjusting the pH of the mixed solution to 5.0 to 6.0, continuing to add laccase, raising the temperature to 60 to 70° C., and reacting for 5 to 7 hours; after the reaction is completed, raising the temperature to 75 to 80° C.

3. The method for preparing Chinese medicinal pieces according to claim 1, wherein: The enzymatic agent includes cellulase and laccase, and the mass ratio of the cellulase to the laccase is 1:3.3-5.0; the method for adding the enzymatic agent is: adjusting the pH of the mixture to 5.0-6.0, adding cellulase, raising the temperature to 45-60°C, and reacting for 5-7 hours; keeping the pH of the mixed solution unchanged, continuing to add laccase, raising the temperature to 60-70°C, and reacting for 3-5 hours; after the reaction is completed, adjusting the pH of the mixed solution to 7.0-8.

0.

4. The method for preparing Chinese medicinal pieces according to claim 1, wherein: In step 1, the method for processing the dry stem of Dendrobium is as follows: clean the dry stem of Dendrobium, dry the surface moisture, cut it into sections of 0.4 cm to 0.8 cm, and grind it to a particle size of 1 to 100 μm to obtain coarse Dendrobium powder.

5. The method for preparing Chinese medicinal pieces according to claim 1, wherein: In step 2, the dendrobium crude powder is poured into deionized water at 25-35° C. according to a solid-liquid ratio of 1:5-10, stirred to form a mixed solution, and stirred continuously for 1-3 hours to fully soak the dendrobium crude powder.

6. The method for preparing Chinese medicinal pieces according to claim 1, wherein: The method of vacuum concentration in step 4 is: vacuum concentrate the filtrate collected in step 3 at a temperature of 40-45° C. and a pressure of 7-12 kPa until the volume becomes 1 / 5-1 / 4 of the original volume.

7. The method for preparing Chinese medicinal pieces according to claim 1, wherein: In step 5, the vacuum freeze-drying step includes the following: In the pre-freezing stage, the temperature is -40 to -50°C for 2 to 5 hours to quickly freeze the dendrobium powder; Primary drying: temperature -15~-30℃, vacuum degree 10~50Pa, time 15~20h, remove surface moisture; Secondary drying: gradually increase the temperature to 20-40°C, vacuum degree 1-10 Pa, time 4-8h, to remove crystal water.

8. The method for preparing Chinese medicinal pieces according to claim 1, wherein: In step six, by weight, 60 to 80 parts of dendrobium powder, 8 to 10 parts of red date powder, and 3 to 5 parts of wolfberry powder are used; the preparation method of the red date powder comprises: grinding and peeling the dried red dates, and then crushing them into red date powder with a particle size of 1 to 20 μm; the particle size of the wolfberry powder is 1 to 20 μm.

9. The method for preparing Chinese medicinal pieces according to claim 1, wherein: In step six, the step of pressing into tablets includes: mixing dendrobium powder, red date powder and wolfberry powder in a proportion to form a mixed powder, using a tablet press to press the mixed powder under a pressure of 10 to 20 kN to form tablets, and the specification of the tablets is 0.5 to 1.0 g / tablet.

Citation Information

Patent Citations

  • Herba dendrobii officinale decoction pieces and processing method thereof

    CN108310228A