Preparation method and application of cordyceps militaris composite wall-broken preparation

By combining physical wall breaking technologies such as circulating freeze-thaw and ball milling, the cell wall and lipids are dissolved, and Cordyceps complex wall breaking preparation with high extraction rate is prepared, which solves the problem of poor absorption and utilization of traditional Chinese medicinal materials in the prior art, and achieves the realization of the problem of loss and poor absorption and utilization of traditional Chinese medicinal materials. It can effectively dissolute and absorb active substances.

CN119453482AInactive Publication Date: 2025-02-18ZHEJIANG GUOBEN PHARM GRP CO LTD
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Patent Information

Application Number
CN202411622114.X
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-14
Publication Date
2025-02-18
Estimated Expiration
Not applicable · inactive patent

AI Technical Summary

Technical Problem

The existing decoction methods of Cordyceps and other medicinal materials are prone to destroy heat-sensitive ingredients, and the decoction of active ingredients is incompletely leading to the loss of ingredients, affecting the body's absorption and utilization.

Method used

A combination of a variety of physical wall breaking techniques, including circulating freeze-thaw and ball milling, dissolve cell walls and lipids through ethanol solution, further break the wall and dissolve active substances, and prepare a composite wall breaking preparation with high extraction rate.

Benefits of technology

It achieves efficient wall breaking, improves the dissolution rate of active substances and the effectiveness of the preparation, and promotes the direct absorption and utilization of drug ingredients.

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Abstract

According to the preparation method and application of the cordyceps militaris composite wall-broken preparation, multiple physical wall-breaking technologies are reasonably utilized and combined, cell walls can be destroyed in different modes, the high wall-breaking rate is achieved, active substances of raw materials are efficiently dissolved out, and the effect of breaking the wall is achieved. The wall-broken preparation with high flavonoid substance and saponin substance content is prepared; according to the method, cell walls of the raw materials are partially or completely destroyed repeatedly in a circulating freezing and thawing manner, so that part of active substances are released, then the cell walls are further destroyed by utilizing ball milling, and the added ethanol can dissolve and destroy lipid in the cell walls and cells, so that the wall breaking effect is further enhanced; and the ethanol solution can also dissolve the released organic active substances, such as flavonoid substances and saponin substances thereof, so that a certain solvent effect is achieved, and the release of the flavonoid substances and the saponin substances thereof can be further facilitated.
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Description

Technical Field

[0001] The present invention relates to the technical field of traditional Chinese medicines, and in particular to a preparation method and application of a Cordyceps militaris composite wall-broken preparation. Background Art

[0002] Cordyceps militaris, ginseng, Saussurea involucrata are all traditional Chinese medicinal materials of the same origin of medicine and food, have the value of food and medicine, it all contains abundant active substances, for example, materials such as flavonoids and saponins thereof, flavonoids have the effects such as improving blood circulation, anti-fatigue, improving immunity, saponins have the effects such as expectorant and relieving cough, invigorating the spleen and replenishing qi, promoting blood circulation and activating collaterals, relieving fatigue, improving immunity. But the medicinal materials such as current Cordyceps militaris, ginseng, Saussurea involucrata mostly are eaten by the traditional method of decoction, not only are easy to destroy its heat-sensitive component, for example, flavonoids, and the effective component decoction is incomplete, can cause the loss of effective ingredients. Although also can be made into powder, it is unfavorable for the direct absorption and utilization of component by body. Summary of the invention

[0003] Therefore, based on the above background, the present invention provides a method for preparing a composite wall-broken preparation of Cordyceps militaris and its application, which utilizes a reasonable combination of multiple physical wall-breaking technologies to prepare a composite wall-broken preparation with a high extraction rate of active substances.

[0004] The technical solution provided by the present invention is:

[0005] A method for preparing a Cordyceps militaris composite wall-broken preparation, the preparation comprising the following steps:

[0006] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively, and passing through a 100-500 mesh sieve;

[0007] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0008] S2: soaking the powder obtained in step S1 with water and then subjecting it to a freeze-thaw cycle;

[0009] S3: After the material has been subjected to freeze-thaw cycles in step S2, an ethanol solution is added and then ground;

[0010] S4: After filtering the material obtained after grinding, taking the filtrate and spray drying it.

[0011] Furthermore, the composition weight ratio of the raw materials is as follows:

[0012] 10-20 parts of Cordyceps militaris, 5-10 parts of ginseng, and 15-30 parts of Saussurea involucrata.

[0013] Furthermore, the freeze-thaw cycle in step S2 is: cooling the water-containing powder to -20°C to -10°C, freezing it for 5-30 minutes, then returning it to room temperature, keeping it for 15-30 minutes, and repeating the cycle 2-8 times.

[0014] Furthermore, in step S2, the powder is soaked with water until water drips out when squeezed.

[0015] Furthermore, the amount of ethanol solution added in step S3 is 3-10 times the weight of the material.

[0016] Furthermore, in step S3, the grinding temperature using a tissue grinder is controlled below 10°C.

[0017] Furthermore, the particle size of the ball milling beads used for the intermediate grinding in step S3 is 0.1-2 mm, and the weight ratio of the ball milling beads to the material after adding ethanol is (2-5):1.

[0018] Based on the same inventive concept, the present invention applies the Cordyceps militaris composite wall-broken preparation prepared by the above method to the preparation of products for improving immunity and resisting fatigue.

[0019] Furthermore, the products include food, beverages, and tea.

[0020] The above technical solution has the following beneficial effects:

[0021] The present invention rationally utilizes a variety of physical cell wall breaking technologies in combination, and can destroy the cell wall in different ways to achieve a high cell wall breaking rate, so that the active substances in the raw materials are efficiently dissolved, so as to efficiently prepare cell wall breaking preparations;

[0022] In the present invention, the cell wall of the raw material is firstly partially or completely destroyed repeatedly in a cyclic freeze-thaw manner to release part of the active substances, and then the cell wall is further destroyed by ball milling, and the added ethanol can dissolve the lipids in the broken cell wall and the broken cells, further enhancing the wall-breaking effect, and the ethanol solution can also dissolve the released organic active substances, such as flavonoids and saponins, etc., play a certain role as a solvent, can further facilitate the release of the active substances, and efficiently prepare the wall-breaking preparation. DETAILED DESCRIPTION

[0023] In order to make the purpose, technical solution and advantages of the embodiments of the present invention clearer, the technical solution in the embodiments of the present invention will be clearly and completely described below in combination with the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0024] The technical solution of the present invention:

[0025] A method for preparing a Cordyceps militaris composite wall-broken preparation, the preparation comprising the following steps:

[0026] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively, and passing through a 100-500 mesh sieve;

[0027] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0028] S2: soaking the powder obtained in step S1 with water and then subjecting it to a freeze-thaw cycle;

[0029] In this step, the powder is soaked with water until water drops out when squeezed, for example, the powder is held in the hand and squeezed until water drops out.

[0030] The freeze-thaw cycle in this step is as follows:

[0031] The water-containing powder is cooled to -20°C to -10°C and then frozen for 5-30 minutes. Then, it is warmed to room temperature and kept for 15-30 minutes. This cycle is repeated 2-8 times.

[0032] S3: After the material has been subjected to freeze-thaw cycles in step S2, an ethanol solution is added and then ground;

[0033] In this step, the amount of ethanol solution added is 3-10 times the weight of the material, and the ethanol has a volume content of 75%.

[0034] In this step, the grinding temperature of the tissue grinder is controlled below 10°C.

[0035] The particle size of the ball milling beads used for grinding is 0.1-2 mm, and the weight ratio of the ball milling beads to the material after adding ethanol is (2-5):1.

[0036] The grinding time of this step is 0.5-5h.

[0037] S4: After filtering the material obtained after grinding, taking the filtrate and spray drying it.

[0038] In this step, a homogenization operation is performed before spray drying, and the air outlet temperature of the sprayer is 60-70°C.

[0039] The composition weight ratio of the raw materials is as follows:

[0040] 10-20 parts of Cordyceps militaris, 5-10 parts of ginseng, and 15-30 parts of Saussurea involucrata.

[0041] The ginseng is taken from 4-year-old ginseng.

[0042] The filtration in this step is performed using a membrane with a pore size of 1 μm.

[0043] Example 1: A method for preparing a composite wall-broken preparation of Cordyceps militaris, the preparation comprising the following steps:

[0044] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively and passing them through a 100-mesh sieve;

[0045] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0046] S2: soaking the powder obtained in step S1 with water and then subjecting it to a freeze-thaw cycle;

[0047] In this step, the powder is soaked with water until water drops out when squeezed, for example, the powder is held in the hand and squeezed until water drops out.

[0048] The freeze-thaw cycle in this step is as follows:

[0049] The water-containing powder was cooled to -15°C and frozen for 30 minutes, then warmed to room temperature and kept for 15 minutes, repeating the cycle twice.

[0050] S3: After the material has been subjected to freeze-thaw cycles in step S2, an ethanol solution is added and then ground;

[0051] In this step, the amount of ethanol solution added is 8 times the weight of the material, and the ethanol has a volume content of 75%.

[0052] In this step, the grinding temperature of the tissue grinder is controlled below 10°C.

[0053] The particle size of the ball milling beads used for grinding is 0.5 mm, and the weight ratio of the ball milling beads to the material after adding ethanol is 3:1.

[0054] The grinding time of this step is 2.5h.

[0055] S4: After filtering the material, take the filtrate and spray dry it.

[0056] In this step, a homogenization operation is performed before spray drying, and the air outlet temperature of the sprayer is 60-70°C.

[0057] The composition weight ratio of the raw materials is as follows:

[0058] Cordyceps militaris 15g, ginseng 10g, snow lotus 20g.

[0059] The ginseng is taken from 4-year-old ginseng.

[0060] Example 2: A method for preparing a composite wall-broken preparation of Cordyceps militaris, the preparation comprising the following steps:

[0061] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively and passing them through a 100-mesh sieve;

[0062] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0063] S2: soaking the powder obtained in step S1 with water and then subjecting it to a freeze-thaw cycle;

[0064] In this step, the powder is soaked with water until water drops out when squeezed, for example, the powder is held in the hand and squeezed until water drops out.

[0065] The freeze-thaw cycle in this step is as follows:

[0066] The powder containing water is cooled to -15°C and then frozen for 30 minutes, then warmed to room temperature and kept for 15 minutes, and the cycle is repeated 5 times. S3: After the material has undergone freeze-thaw cycles in step S2, the ethanol solution is added and then ground;

[0067] In this step, the amount of ethanol solution added is 8 times the weight of the material, and the ethanol has a volume content of 75%.

[0068] In this step, the grinding temperature of the tissue grinder is controlled below 10°C.

[0069] The particle size of the ball milling beads used for grinding is 0.5 mm, and the weight ratio of the ball milling beads to the material after adding ethanol is 3: 1. The grinding time of this step is 2.5 hours.

[0070] S4: After filtering the material, take the filtrate and spray dry it.

[0071] In this step, a homogenization operation is performed before spray drying, and the air outlet temperature of the sprayer is 60-70°C.

[0072] The composition weight ratio of the raw materials is as follows:

[0073] Cordyceps militaris 15g, ginseng 10g, snow lotus 20g.

[0074] The ginseng is taken from 4-year-old ginseng.

[0075] Example 3: A method for preparing a composite wall-broken preparation of Cordyceps militaris, the preparation comprising the following steps:

[0076] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively, and passing through a 100-500 mesh sieve;

[0077] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0078] S2: soaking the powder obtained in step S1 with water and then subjecting it to a freeze-thaw cycle;

[0079] In this step, the powder is soaked with water until water drops out when squeezed, for example, the powder is held in the hand and squeezed until water drops out.

[0080] The freeze-thaw cycle in this step is as follows:

[0081] The powder containing water is cooled to -15°C and then frozen for 30 minutes, then warmed to room temperature and kept for 15 minutes, and the cycle is repeated 8 times. S3: After the material has undergone freeze-thaw cycles in step S2, the ethanol solution is added and then ground;

[0082] In this step, the amount of ethanol solution added is 8 times the weight of the material, and the ethanol has a volume content of 75%.

[0083] In this step, the grinding temperature of the tissue grinder is controlled below 10°C.

[0084] The particle size of the grinding ball beads is 0.5 mm, and the weight ratio of the ball beads to the material after adding ethanol is 3: 1. S4: After filtering the material, take the filtrate and spray dry it.

[0085] In this step, a homogenization operation is performed before spray drying, and the air outlet temperature of the sprayer is 60-70°C.

[0086] The composition weight ratio of the raw materials is as follows:

[0087] Cordyceps militaris 15g, ginseng 10g, snow lotus 20g.

[0088] The ginseng is taken from 4-year-old ginseng.

[0089] Comparative Example 1: A method for preparing a composite wall-broken preparation of Cordyceps militaris, the preparation comprising the following steps:

[0090] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively, and passing through a 100-500 mesh sieve;

[0091] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0092] S2: soaking the powder obtained in step S1 with water, adding ethanol solution, and grinding;

[0093] In this step, the amount of ethanol solution added is 5 times the weight of the material, and the ethanol has a volume content of 75%.

[0094] In this step, the grinding temperature of the tissue grinder is controlled below 10°C.

[0095] The particle size of the ball milling beads used for grinding is 0.5 mm, and the weight ratio of the ball milling beads to the material after adding ethanol is 3: 1. The grinding time of this step is 12 hours.

[0096] S3: After filtering the material, take the filtrate and spray dry it.

[0097] In this step, a homogenization operation is performed before spray drying, and the air outlet temperature of the sprayer is 60-70°C.

[0098] The composition weight ratio of the raw materials is as follows:

[0099] Cordyceps militaris 15g, ginseng 10g, snow lotus 20g.

[0100] The ginseng is taken from 4-year-old ginseng.

[0101] Comparative Example 2: A method for preparing a composite wall-broken preparation of Cordyceps militaris, the preparation comprising the following steps:

[0102] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively, and passing through a 100-500 mesh sieve;

[0103] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0104] S2: soaking the powder obtained in step S1 with water and then subjecting it to a freeze-thaw cycle;

[0105] In this step, the powder is soaked with water until water drops out when squeezed, for example, the powder is held in the hand and squeezed until water drops out.

[0106] The freeze-thaw cycle in this step is as follows:

[0107] The water-containing powder is cooled to -15°C and then frozen for 30 minutes, then warmed to room temperature and kept for 15 minutes, and the cycle is repeated 5 times. S3: After the material has undergone freeze-thaw cycles in step S2, the ethanol solution is added and homogenized.

[0108] S4: After filtering the material, take the filtrate and spray dry it.

[0109] In this step, homogenization is performed before spray drying.

[0110] The composition weight ratio of the raw materials is as follows:

[0111] Cordyceps militaris 15g, ginseng 10g, snow lotus 20g.

[0112] The ginseng is taken from 4-year-old ginseng.

[0113] Comparative Example 3: A method for preparing a composite wall-broken preparation of Cordyceps militaris, the preparation comprising the following steps:

[0114] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively, and passing through a 100-500 mesh sieve;

[0115] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0116] S2: adding ethanol solution to the powder obtained in step S1 and grinding;

[0117] In this step, the amount of ethanol solution added is 5 times the weight of the material, and the ethanol has a volume content of 75%.

[0118] In this step, the grinding temperature of the tissue grinder is controlled below 10°C.

[0119] The particle size of the ball milling beads used for grinding is 0.5 mm, and the weight ratio of the ball milling beads to the material after adding ethanol is 3: 1. The grinding time of this step is 2.5 hours.

[0120] S3: The material ground in step S2 is subjected to a freeze-thaw cycle.

[0121] The freeze-thaw cycle in this step is as follows:

[0122] The water-containing powder was cooled to -15°C and frozen for 30 minutes, then warmed to room temperature and kept for 15 minutes. This cycle was repeated 5 times.

[0123] S4: After filtering the material, take the filtrate and spray dry it.

[0124] In this step, a homogenization operation is performed before spray drying, and the air outlet temperature of the sprayer is 60-70°C.

[0125] The composition weight ratio of the raw materials is as follows:

[0126] Cordyceps militaris 15g, ginseng 10g, snow lotus 20g.

[0127] The ginseng is taken from 4-year-old ginseng.

[0128] Comparative Example 4: A method for preparing a composite wall-broken preparation of Cordyceps militaris, the preparation comprising the following steps:

[0129] S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively, and passing through a 100-500 mesh sieve;

[0130] The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata;

[0131] S2: soaking the powder obtained in step S1 with water and then subjecting it to a freeze-thaw cycle;

[0132] In this step, the powder is soaked with water until water drops out when squeezed, for example, the powder is held in the hand and squeezed until water drops out.

[0133] The freeze-thaw cycle in this step is as follows:

[0134] The water-containing powder was cooled to -15°C and frozen for 30 minutes, then warmed to room temperature and kept for 15 minutes. This cycle was repeated 5 times.

[0135] S3: After the freeze-thaw cycle in step S2, water is added to the material and then ground;

[0136] The amount of water added in this step is 5 times the weight of the material.

[0137] In this step, the grinding temperature of the tissue grinder is controlled below 10°C.

[0138] The particle size of the ball milling beads used for grinding is 0.5 mm, and the weight ratio of the ball milling beads to the material after adding ethanol is 3:1.

[0139] The grinding time of this step is 2.5h.

[0140] S4: After filtering the material, take the filtrate and spray dry it.

[0141] In this step, a homogenization operation is performed before spray drying, and the air outlet temperature of the sprayer is 60-70°C.

[0142] The composition weight ratio of the raw materials is as follows:

[0143] Cordyceps militaris 15g, ginseng 10g, snow lotus 20g.

[0144] The ginseng is taken from 4-year-old ginseng.

[0145] The yields of the cell wall-broken preparations prepared in Examples 1 to 3 and Comparative Examples 1 to 4 can be seen in the table below.

[0146] The particles of the broken wall preparation finally prepared in the above embodiment and its comparative example are highly soluble organic active substances in the extract, and the final yield of the broken wall preparation can reflect the release of the organic active substances.

[0147] The test results are shown in the table below:

[0148] Example 1 Example 2 Example 3 Comparative Example 1 Comparative Example 2 Comparative Example 3 Comparative Example 4 Production of wall-breaking agent 7.37 11.25 13.59 5.24 3.86 9.12 9.85

[0149] The present invention and its implementation methods are described above, and such description is not restrictive, and the actual methods are not limited thereto. In short, if ordinary technicians in the field are inspired by it, without departing from the purpose of the invention, they can design implementation methods and embodiments similar to the technical solution without creativity, which should all fall within the protection scope of the present invention.

Claims

1. A method for preparing a composite wall-broken preparation of Cordyceps militaris, characterized in that: Its preparation comprises the following steps: S1: taking raw materials according to the amount and mixing them, crushing the raw materials respectively, and passing through a 100-500 mesh sieve; The raw materials are composed of Cordyceps militaris, Ginseng and Saussurea involucrata; S2: soaking the powder obtained in step S1 with water and then subjecting it to a freeze-thaw cycle; S3: After the material has been subjected to freeze-thaw cycles in step S2, an ethanol solution is added and then ground; S4: After filtering the material obtained after grinding, taking the filtrate and spray drying it.

2. The method for preparing a Cordyceps militaris composite wall-broken preparation according to claim 1, characterized in that: The composition weight ratio of the raw materials is as follows: 10-20 parts of Cordyceps militaris, 5-10 parts of ginseng, and 15-30 parts of Saussurea involucrata.

3. The method for preparing a Cordyceps militaris composite wall-broken preparation according to claim 1, characterized in that: The freeze-thaw cycle in step S2 is as follows: the water-containing powder is cooled to -20°C to -10°C and then frozen for 5-30 minutes, then warmed to room temperature and kept for 15-30 minutes, and the cycle is repeated 2-8 times.

4. The method for preparing a composite wall-broken preparation of Cordyceps militaris according to claim 1, characterized in that: In step S2, the powder is soaked with water until water drips out when squeezed.

5. The method for preparing a Cordyceps militaris composite wall-broken preparation according to claim 1, characterized in that: The amount of ethanol solution added in step S3 is 3-10 times the weight of the material.

6. The method for preparing a Cordyceps militaris composite wall-broken preparation according to claim 1, characterized in that: The grinding temperature in step S3 is controlled below 10°C.

7. The method for preparing a Cordyceps militaris composite wall-broken preparation according to claim 1, characterized in that: The particle size of the ball milling beads used for the intermediate grinding in step S3 is 0.1-2 mm, and the weight ratio of the ball milling beads to the material after adding ethanol is (2-5):

1.

8. Use of the Cordyceps militaris composite broken wall preparation prepared by the method for preparing the Cordyceps militaris composite broken wall preparation according to any one of claims 1 to 7, characterized in that: The Cordyceps militaris composite wall-broken preparation is used for preparing products for improving immunity and resisting fatigue.

9. The use according to claim 8, characterized in that: The products include food, beverages and tea.