CN113476890A

CN113476890A - Wet grinding traditional Chinese medicine extraction method and wet grinding traditional Chinese medicine extraction device

Info

Publication number: CN113476890A
Application number: CN202110846402.3A
Authority: CN
Inventors: 曾浩然
Original assignee: Guangzhou Biogreen Biotechnology Co ltd
Current assignee: Guangzhou Biogreen Biotechnology Co ltd
Priority date: 2021-07-26
Filing date: 2021-07-26
Publication date: 2021-10-08

Abstract

The invention discloses a wet-method crushed traditional Chinese medicine extraction method and a wet-method crushed traditional Chinese medicine extraction device, and relates to the technical field of traditional Chinese medicine extraction. The wet grinding traditional Chinese medicine extraction method comprises the following steps: putting the traditional Chinese medicinal materials to be extracted into crushing equipment, and introducing water vapor into the crushing equipment to extract while crushing; wherein the temperature of the water vapor is 40-100 ℃. The inventor creatively extracts the Chinese medicinal materials in a crushing device, introduces water vapor with the temperature of 40-100 ℃ to mix and extract the Chinese medicinal materials, and can crush the particle size of the Chinese medicinal materials to a finer level through the crushing device, thereby obviously shortening the extraction time. More importantly, the high-temperature steam is contacted with the traditional Chinese medicinal materials to be extracted for extraction, so that the traditional Chinese medicinal materials are not heated in the extraction process, unpleasant odor generated by heating is prevented, effective components such as volatile oil are retained to a greater extent, and the traditional Chinese medicinal materials have good market application prospect.

Description

Wet grinding traditional Chinese medicine extraction method and wet grinding traditional Chinese medicine extraction device

Technical Field

The invention relates to the technical field of traditional Chinese medicine extraction, in particular to a wet grinding traditional Chinese medicine extraction method and a wet grinding traditional Chinese medicine extraction device.

Background

The traditional Chinese medicine generally needs to be decocted for a long time to extract effective components, but the traditional Chinese medicine is decocted at home for a long time by a patient, so that a plurality of patients are forbidden to the complicated traditional Chinese medicine decoction.

At present, some decocting machines special for traditional Chinese medicines exist. For example, CN201520639361 describes that the heating extraction of medicinal materials is performed by electricity, advocates that the small-sized traditional Chinese medicine decocting machine replaces open fire, can control the heating temperature in the decocting process according to a temperature display and a control panel, and does not get rid of the traditional water decocting method. CN 201820171766A Chinese medicinal decoction machine is based on the former, and is added with a function of squeezing Chinese medicinal residue.

The current medicine decocting machine generally has the following problems: (1) the decoction time is long; (2) long-time heating easily causes the decomposition of the drug effect components; (3) the retention of components such as volatile oil is low.

In view of this, the invention is particularly proposed.

Disclosure of Invention

The invention aims to provide a wet grinding traditional Chinese medicine extraction method, which aims to remarkably shorten the extraction time, better retain effective components and avoid unpleasant smell of decoction.

The invention also aims to provide a wet grinding traditional Chinese medicine extraction device which is simple to operate, short in extraction time and high in extraction rate of effective components.

The invention is realized by the following steps:

in a first aspect, the invention provides a wet grinding traditional Chinese medicine extraction method, which comprises the steps of placing traditional Chinese medicines to be extracted in grinding equipment, introducing water vapor into the grinding equipment, and extracting while grinding;

wherein the temperature of the water vapor is 40-100 ℃.

In a second aspect, the present invention provides a wet-milling chinese medicine extraction apparatus for carrying out the extraction method of any one of the preceding embodiments, comprising a steam generator for generating steam for extraction and a milling device for performing the extraction, the steam outlet of the steam generator being in communication with the air inlet of the milling device.

The invention has the following beneficial effects: the inventor creatively extracts the Chinese medicinal materials in a crushing device, introduces water vapor with the temperature of 40-100 ℃ to mix and extract the Chinese medicinal materials, and can crush the particle size of the Chinese medicinal materials to a finer level through the crushing device, thereby obviously shortening the extraction time. More importantly, the high-temperature steam is contacted with the traditional Chinese medicinal materials to be extracted for extraction, so that the traditional Chinese medicinal materials are not heated in the extraction process, unpleasant odor generated by heating is prevented, effective components such as volatile oil are retained to a greater extent, and the traditional Chinese medicinal materials have good market application prospect.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.

Fig. 1 is a schematic view of a wet grinding traditional Chinese medicine extraction device provided in an embodiment of the present invention;

FIG. 2 is an electron microscope image of the extracted Chinese medicinal material 1 in example 1;

FIG. 3 is an electron microscope image of the extracted Chinese medicinal material 2 of example 2;

FIG. 4 is a liquid phase fingerprint of decoction extracted from the Chinese herbal medicine 3 in the example;

FIG. 5 is a liquid fingerprint of decoction obtained by extracting herb 3 by conventional decoction;

FIG. 6 is a comparison of particle sizes of conventional dry milled and wet ultra fine D50 particles;

FIG. 7 is a comparison of cumulative% dissolution of protein;

FIG. 8 is a graph showing the results of the measurement of the size of the ultrafine powder particles obtained by the wet method with time.

Icon: 100-a wet grinding traditional Chinese medicine extraction device; 110-a steam generator; 120-a crushing device; 130-a filter assembly; 131-mesh screen; 132-ceramic membrane.

Detailed Description

In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.

The conventional traditional Chinese medicine decoction process is an operation of extracting soluble components in the traditional Chinese medicine solid raw materials by using water as a solvent. The scientific nature of the method is the mass transfer process of solute from solid phase to liquid phase. The extraction process can be generally divided into 3 steps: (1) penetration of solvent into the medicinal material and moistening the medicinal material; (2) dissolving solute in the medicinal material; (3) the diffusion of solute from the inside of the medicinal material to the surface of the medicinal material and from the surface of the medicinal material to the main body of the solution.

The embodiment of the invention provides a method for extracting a traditional Chinese medicine by wet grinding, which comprises the steps of putting a traditional Chinese medicine to be extracted into grinding equipment, introducing water vapor into the grinding equipment, and extracting while grinding; wherein the temperature of the water vapor is 40-100 ℃.

The inventor improves the extraction mode of the traditional Chinese medicinal materials, utilizes high-temperature steam to be instantly contacted and heated with the traditional Chinese medicinal materials to be extracted, extracts the traditional Chinese medicinal materials while crushing the traditional Chinese medicinal materials, has no heat source supply in the extraction process, and mainly has the following advantages:

(1) the particle size of the traditional Chinese medicinal materials can be obviously reduced by using crushing equipment, even the particle size can reach the cell level, the diffusion resistance can be reduced, the component dissolution path can be shortened, the dissolution area can be increased, the rapid and complete dissolution of effective components can be facilitated, and the extraction time can be obviously shortened;

(2) the continuous heating of a heat source does not exist in the extraction process, so that the problems of gelatinization, wall sticking, difficult filtration and the like caused by long-time decoction are avoided;

(3) can remarkably improve the extraction rate of effective components such as volatile oil.

It is necessary to supplement that if the dry-type superfine grinding technology is adopted, the medicinal materials are crushed to the cell level and then decocted by adding water, although the extraction efficiency is improved, the problems of gelatinization, wall adhesion, difficult filtration and the like caused by too small particle size of medicinal material particles during decoction are often caused, and the process cannot be industrialized. The traditional Chinese medicine decoction system in the embodiment of the application follows the concept of 'keeping right and creating new' of the modernization of traditional Chinese medicine, and inherits the 'decoction' method of the traditional Chinese medicine insisting, and the traditional Chinese medicine is contacted with high-temperature water vapor in a short time at the moment of crushing, and the preparation of the traditional Chinese medicine decoction is completed within 10 minutes.

Specifically, the temperature of the water vapor is determined according to the type of the medicinal material to be extracted, and may be 40 ℃, 50 ℃, 60 ℃, 70 ℃, 80 ℃, 90 ℃, 100 ℃ or the like, or may be any value between the above adjacent temperature values.

Further, the mass ratio of the Chinese medicinal materials to be extracted to the introduced water vapor is 1: 8-12; preferably 1: 9-11. The extraction efficiency is further improved by regulating the mass ratio of the Chinese medicinal materials to be extracted to the steam. Specifically, the mass ratio of the traditional Chinese medicinal materials to be extracted to the introduced water vapor can be 1:8, 1:9, 1:10, 1:11, 1:12 and the like, and can also be any value between the adjacent mass ratios.

In some embodiments, the water vapor is introduced by atomized spray; the required steam is generated using a steam generator that instantaneously generates high pressure and heats water, and the steam is injected into the pulverizing apparatus. The term "instant" refers to that water can be heated to steam instantly, and a certain pressure is applied, and the steam is sprayed into the wet superfine grinding equipment and contacts with the medicinal materials for a short time. The injection rate of the water vapor is 5-300mL/min, preferably 100-200mL/min, such as 5mL/min, 50mL/min, 100mL/min, 150mL/min, 200mL/min, 250mL/min, 300mL/min, etc.

Furthermore, the crushing equipment is wet ultrafine crushing equipment, so that the traditional Chinese medicinal material to be extracted is crushed to the central particle size of below 5-10 mu m in the extraction process, and the rotating speed is controlled to be 100-3000 rpm; preferably 500-. The dry-method superfine grinding process can grind the materials to the central particle size of 150-200 meshes (more than 75 mu m), and the wet-method grinding process can grind the traditional Chinese medicinal materials to a finer level. Under the condition of the fineness, the wall-broken rate of the cells of the general medicinal materials is more than 95 percent, once the cell walls are broken in the crushing process, the surfaces of the micro-particles can form a semi-moist state after the water and oil in the cells are migrated out, semi-stable particle groups are formed among the particles, and the insoluble components in the Chinese medicinal materials can be quickly and efficiently dissolved out.

It is necessary to supplement that the wet superfine grinding is an extension of the dry superfine grinding technology, belongs to the prior art, but is not used in the extraction of the traditional Chinese medicinal materials. The technology can make solvent reach the inside of plant tissue while crushing, and uses strong mechanical vibration to grind the tissue, so that the effective components in the tissue are dissolved in the solvent, thereby achieving the purpose of rapid and effective extraction. In the wet superfine grinding extraction process, the dissolution of the active ingredients has the advantages of small diffusion resistance, short dissolution path and large dissolution area. In addition, the medicinal material particles absorbed with the solvent are continuously sheared and extruded by mechanical force until cell-level crushing is achieved, the convection of the solvent is greatly increased by the mechanical force, the mass transfer coefficient is improved, the effective components are promoted to be rapidly transferred to the solvent, the extraction process which usually needs several hours is shortened to dozens of minutes, and the extraction efficiency is greatly improved.

Further, the extraction time is 5-20min, preferably 10-15 min. In the actual operation process, the material to be extracted is added into a wet superfine grinding device, and is instantaneously contacted with high-temperature steam while being ground, and the traditional Chinese medicine decoction can be obtained through short-time extraction. Specifically, the extraction time may be 5min, 10min, 15min, 20min, or the like, or may be any value between the above adjacent time values.

In some embodiments, the resulting herbal decoction is filtered after extraction is complete, removing impurities and unpleasant foam from the liquid. The filtering is carried out by adopting a mesh screen and then filtering by using a ceramic membrane, wherein the aperture of the adopted mesh screen is 0.1-5.0mm (namely the size of the mesh in the mesh screen), and the aperture of the micro-filtration ceramic membrane is 0.2-2.0 mu m.

It should be added that the wet grinding traditional Chinese medicine extraction method provided by the embodiment of the invention can be used for treating the traditional Chinese medicine fresh medicines which need to be taken by fresh juicing, such as fresh lotus leaves, fresh reed rhizome, fresh bamboo shavings, honeysuckle flower syrup, fresh calamus, fresh watermelon white juice, fresh rehmannia root juice and related compounds, such as Qianjin Yao Fang: raw lophatherum gracile, raw bamboo shavings, raw folium artemisiae argyi (below the three women), and the like.

Due to the high cost of culture, storage and transportation of fresh medicines and the backward preservation technology of medicinal materials, the fresh medicines are difficult to be widely used in modern clinic. The invention can effectively break the technical bottleneck of popularization and application of the fresh traditional Chinese medicine in the modern society. The fresh traditional Chinese medicine has the characteristics of pure fresh medicine juice and good smell by adopting the extraction method in the embodiment of the invention, and can maintain the natural performance of the medicine to the maximum extent, maintain the biological activity of the medicine and achieve the aim of fresh use.

Referring to fig. 1, an embodiment of the present invention further provides a wet grinding traditional Chinese medicine extracting apparatus 100, which includes a steam generator 110 for generating steam for extraction and a grinding device 120 for extraction, wherein a steam outlet of the steam generator 110 is communicated with an air inlet of the grinding device 120. Steam is generated by the steam generator 110 and passed into the milling apparatus 120 as a solvent for extraction.

It should be noted that the steam generator 110 and the crushing device 120 may be existing devices, and are not limited herein.

In some embodiments, the steam generator 110 may be an instant high temperature and high pressure steam generator, which can instantly heat water to steam and add a certain pressure, and can instantly spray a small amount of steam, such as 5mL to 100 mL. The pulverizing device 120 may be a wet ultrafine pulverizer, which is used as an extraction kettle to perform extraction while pulverizing. By utilizing the coupling of instantaneous high-temperature and high-pressure steam and wet superfine extraction, the steam sprayed instantaneously can further accelerate the wet superfine grinding extraction speed, and the excessive extraction caused by the long-time contact of the traditional Chinese medicine liquid with a heat source is also avoided.

Specifically, the wet ultrafine pulverizer can pulverize the medicinal materials to 5-5000 μm in the state of coexistence of the medicinal materials and the solvent, and can control the pulverizing time and pulverizing mode by circuit, and can be continuous or intermittent.

In the actual working process, the instantaneous high-temperature and high-pressure water vapor generator can pressurize to 1-6bar in the generator, instantaneously heat water to 80-110 ℃, and the temperature and the duration time can be flexibly controlled through frequency. The function can fully reflect the principle of 'keeping right and inheriting' of traditional Chinese medicine scientific research, comprehensively adapt to the requirements of special decocting methods such as 'decocting first', 'then decocting down' and the like in the traditional Chinese medicine theory, and are controlled by components such as a panel control button and the like: (1) the traditional Chinese medicine varieties needing to be processed later, such as scutellaria baicalensis, bitter apricot seeds and the like, are subjected to 'enzyme deactivation and glycoside protection' operation in advance so as to kill biological enzymes in the traditional Chinese medicine materials and prevent the biological enzymes from generating enzymolysis and destroying active ingredients in the heating extraction process; (2) extracting volatile oil from Chinese medicinal materials such as herba Menthae and fructus Amomi by steam distillation, and completely retaining volatile medicinal components such as terpenes, alcohols, aldehydes, and phenols; (3) the Chinese medicine species needing decocting first, such as aconite root, aconite root and other toxic Chinese medicine, is treated through attenuation and synergism to destroy its toxic components at high temperature, and then converted into active components through hydrolysis.

In an alternative embodiment, a filter assembly 130 is further included, the filter assembly 130 is located below the crushing device 120 and faces the discharge port of the crushing device, the filter assembly 130 includes a mesh screen 131 and a ceramic membrane 132, the mesh screen 131 is used for filtering, the filtrate is filtered by the ceramic membrane 132, and the filtered medicament is collected in the lower container by opening the valve.

In the actual operation process, after extraction is completed, the upper instantaneous high-temperature high-pressure water vapor generator can be used for pressing the lower crushing equipment, 0.1-2.5bar of pressure is applied, a valve is opened, the traditional Chinese medicine decoction enters the lower filtering component 130 for refining, separation of drug effect small molecular components and high molecular non-drug effect substances is realized at the molecular level, and the refined components are collected in the traditional Chinese medicine decoction.

The features and properties of the present invention are described in further detail below with reference to examples.

Example 1

The embodiment provides a wet grinding traditional Chinese medicine extraction method, which adopts the device in fig. 1 for extraction and comprises the following steps:

10g of the Chinese medicinal material 1 (ephedra herb) is put into a crushing device (a wet-process ultrafine pulverizer), about 5mL of water vapor with the temperature of 80 ℃ is sprayed into the crushing device by using a steam generator 110, and the crushing device is started at the same time, and the rotating speed is controlled to be 500 rpm.

Controlling the steam injection speed at 5mL/min and the injection weight at 100mL, continuously operating the pulverizing equipment for 20min, applying pressure to the pulverizing equipment to 1.0bar by using the upper steam generator 110, and opening the valve to complete extraction.

The particle size of the extracted crude drug 1 can reach about 20 μm by detection, as shown in fig. 2.

Example 2

50g of the Chinese medicinal material 2 (astragalus) is put into a crushing device (a wet-process ultrafine crusher), about 10mL of water vapor with the temperature of 80 ℃ is sprayed into the crushing device by using a steam generator 110, and the crushing device is started at the same time, and the rotating speed is controlled to be 1000 rpm.

Controlling the steam injection speed at 100mL/min and the injection weight at 500mL, continuously operating the pulverizing equipment for 5min, applying pressure to the pulverizing equipment to 0.50bar by using the upper steam generator 110, and opening the valve to complete extraction.

Through detection, the particle size of the traditional Chinese medicine material 2 after extraction can reach about 300 μm, as shown in figure 3.

Example 3

20g of the Chinese medicinal herb 1 (ephedra herb) is put into a crushing device (a wet-process ultrafine pulverizer), about 8mL of water vapor with the temperature of 90 ℃ is sprayed into the crushing device by a steam generator 110, and the crushing device is started at the same time, and the rotating speed is controlled to be 300 rpm.

Controlling the water vapor injection speed at 40mL/min and the injection weight at 200mL, continuously operating the pulverizing equipment for 5min, applying pressure to the pulverizing equipment to 2.0bar by using the upper steam generator 110, and opening the valve to complete extraction.

Through detection, the final extraction rate is compared with the conventional heating reflux extraction ratio shown in table 1, and the extraction rate of the ephedra is 10 times of that of the conventional heating reflux extraction ratio.

TABLE 1 comparison of extraction rates for different methods

Method	Extraction ratio of Chinese ephedra of medicinal material 1 (%)
		Wet superfine extraction	64.5
Solvent reflux	6.4

Wherein, the operation steps of the conventional heating reflux extraction are as follows: (1) accurately weighing the medicinal materials and the solvent in a weight ratio of 1:10, adding the mixture into a reflux heating device; (2) heating the medicinal materials and solvent to boiling (water as solvent at normal pressure of 100 deg.C), and reflux-extracting; (3) after the set time, pouring out the liquid medicine and separating dregs of a decoction.

Example 4

100g of Chinese medicinal material 3 (scorpion) is put into a crushing device (a wet-process ultrafine crusher), about 50mL of water vapor with the temperature of 80 ℃ is sprayed into the crushing device by a steam generator 110, and the crushing device is started at the same time, and the rotating speed is controlled to be 800 rpm.

Controlling the steam injection speed at 100mL/min and the injection weight at 1000mL, continuously operating the pulverizing equipment for 10min, applying pressure to the pulverizing equipment to 2.5bar by using the upper steam generator 110, and opening the valve to complete extraction.

Through detection, the decoction obtained by the wet ultrafine extraction in the embodiment has extremely high contrast similarity with the traditional Chinese medicine decoction obtained by decocting the traditional Chinese medicine in water for 40 minutes (the dosage of the traditional Chinese medicine and the water is the same as that in the embodiment), as shown in fig. 4 and fig. 5.

Example 5

putting 12g of Chinese medicinal material 4 (Lumbricus) into pulverizing equipment (wet superfine pulverizer), spraying 5mL of 50 deg.C water vapor into the pulverizing equipment by steam generator 110, and simultaneously starting the pulverizing equipment at 500 rpm.

Controlling the steam injection speed at 8mL/min and the injection weight at 120mL, continuously operating the pulverizing equipment for 15min, then applying pressure to the pulverizing equipment to 1.0bar by using the upper steam generator 110, and opening the valve to complete extraction.

The wet ultrafine powder is detected to be finer than the conventional dry-ground powder in the same time (as shown in FIG. 6); the wet ultrafine comminution extracted protein eluted at a significantly higher percentage in the same time period than the conventional dry milling eluted protein (as shown in FIG. 7).

Wherein, the operation of the conventional dry grinding dissolution is as follows:

(1) accurately weighing dry medicinal materials, adding into a pulverizer for pulverizing, and sieving with a second sieve; (2) adding 10 times of water, adding into homogenizer (10000 r.min) together with the medicinal materials^-1) Homogenizing; (3) after the set time, centrifuging and taking supernatant.

Example 6

10g of the Chinese herbal medicine 4 (earthworm) is put into a grinding device (a wet-process ultrafine grinder), about 5mL of water vapor with the temperature of 50 ℃ is sprayed into the grinding device by a steam generator 110, and the grinding device is started at the same time, and the rotating speed is controlled to be 300 rpm.

Controlling the water vapor injection speed at 40mL/min and the injection weight at 100mL, continuously operating the pulverizing equipment for 5min, respectively, applying pressure to the pulverizing equipment to 2.0bar by using the upper steam generator 110, and opening the valve to complete extraction.

Examples 7 to 10

Examples 7-10 differed from example 6 only in that the extraction times were 10min, 15min, 20min, and 30min, respectively.

The particle sizes of the herbs after extraction in examples 6 to 10 were measured, and as a result, as shown in FIG. 8, it was found that the particle sizes of the herbs could not be further reduced by further pulverization after the wet ultrafine pulverization exceeded 20 min. This may be due to the fact that the cell structure has been completely destroyed and the various components of the cell can come into contact with the solvent.

The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A wet grinding traditional Chinese medicine extraction method is characterized by comprising the following steps: putting the traditional Chinese medicinal materials to be extracted into crushing equipment, and introducing water vapor into the crushing equipment to extract while crushing;

wherein the temperature of the water vapor is 40-100 ℃.

2. The wet grinding traditional Chinese medicine extraction method as claimed in claim 1, wherein the mass ratio of the traditional Chinese medicine to be extracted to the introduced water vapor is 1: 8-12; preferably 1: 9-11.

3. The method as claimed in claim 2, wherein the steam is introduced by atomization and injection, and the injection speed of the steam is 5-300mL/min, preferably 100-200 mL/min.

4. The method for extracting a wet-pulverized traditional Chinese medicine as claimed in claim 3, wherein the pulverizing apparatus is a wet ultra-fine pulverizing apparatus to pulverize the traditional Chinese medicine to be extracted to a central particle size of 5-10 μm or less during the extraction process.

5. The method as claimed in claim 4, wherein the rotation speed is controlled to be 100-3000 rpm; preferably 500-.

6. The extraction method of the wet-pulverized traditional Chinese medicine as claimed in claim 1, wherein the extraction time is 5-20min, preferably 10-15 min.

7. The method for extracting a wet-pulverized traditional Chinese medicine as claimed in claim 6, wherein the obtained traditional Chinese medicine decoction is filtered after the extraction is completed.

8. The method for extracting a wet-milled traditional Chinese medicine as claimed in claim 7, wherein the filtration is performed by using a mesh screen and then the filtration is performed by using a ceramic membrane, and the pore size of the mesh screen is 0.1 to 5.0 mm; the aperture of the ceramic membrane is 0.2-2.0 μm.

9. A wet-grinding traditional Chinese medicine extraction device for implementing the extraction method of any one of claims 1 to 8, which is characterized by comprising a steam generator for generating steam for extraction and a grinding device for extraction, wherein a steam outlet of the steam generator is communicated with an air inlet of the grinding device.

10. The extraction device for the wet grinding traditional Chinese medicine as claimed in claim 9, further comprising a filtering component, wherein the filtering component is located below the grinding equipment and faces the discharge hole of the grinding equipment.