Device and method for rapidly separating small molecule compounds in traditional Chinese medicinal materials

Abstract

The invention discloses a device and method for rapidly separating small molecular compounds in traditional Chinese medicinal materials, and relates to the technical field of extraction and separation of traditional Chinese medicinal materials, and the device for rapidly separating the small molecular compounds in the traditional Chinese medicinal materials comprises a material tank, a filter screen, a conveying pipe and a membrane assembly. The material tank is used for containing medicinal materials and solvents, and a discharging opening is formed in the bottom of the material tank; the filter screen is arranged above the discharge hole in a covering manner; one end of the conveying pipe is communicated with the discharge hole of the charging bucket, and a pump is arranged on the conveying pipe; a feeding port of the membrane assembly is communicated with the other end of the conveying pipe, a trapped fluid outlet of the membrane assembly is communicated with the material tank, and the pump can pump liquid medicine in the material tank into the membrane assembly in a starting state. The production cost and the operation difficulty can be reduced, and the production efficiency is improved.

Description

Technical Field

[0001] The present invention relates to the technical field of extraction and separation of traditional Chinese medicine, and in particular to a device and method for rapidly separating small molecule compounds in traditional Chinese medicine. Background Art

[0002] Traditional Chinese medicine refers to substances that are used to prevent, treat, diagnose diseases and have rehabilitation and health-care effects under the guidance of traditional Chinese medicine theory. Traditional Chinese medicine mainly comes from natural medicines and their processed products, including herbal medicines, animal medicines, mineral medicines and some chemical and biological products. For thousands of years, traditional Chinese medicine decoctions, mainly decocted in water, have been the main way of clinical use of traditional Chinese medicine. The components of traditional Chinese medicine water extracts are extremely complex, the content of effective ingredients is generally low, and the molecular weight is generally less than 1000. They often contain non-functional ingredients such as starch, protein, mucus, pigments, gum, pectin, etc., which are the key factors for the large dosage of traditional Chinese medicine preparations, strong hygroscopicity, and difficulty in preparing fast-acting dosage forms. Many traditional Chinese medicine products still show the characteristics of being large, black, and coarse.

[0003] In the production of traditional Chinese medicinal material extracts, there are the following problems: First, the process is complicated and requires a variety of equipment such as extraction equipment, plate and frame filters (centrifuges), evaporators, membrane separation equipment, spray dryers, etc., and the equipment investment is relatively high; Second, the liquid medicine contains a large amount of ineffective ingredients, such as pectin, starch and other high molecular substances, which causes the liquid medicine to have a high viscosity and is difficult to filter. In the subsequent membrane separation operation, the membrane flux decreases rapidly, and the production efficiency is greatly reduced. Summary of the invention

[0004] The purpose of the present invention is to provide a device and method for quickly separating small molecule compounds in Chinese medicinal materials, so as to solve the problems existing in the above-mentioned prior art, reduce production costs and operation difficulty, and improve production efficiency.

[0005] To achieve the above object, the present invention provides the following solutions:

[0006] The present invention provides a device for rapidly separating small molecular compounds in traditional Chinese medicine, comprising:

[0007] A material tank, used to contain medicinal materials and solvents, with a discharge port provided at the bottom of the material tank;

[0008] A filter screen, wherein the filter screen cover is arranged above the discharge port;

[0009] a delivery pipe, one end of which is connected to the discharge port of the material tank, and a pump is provided on the delivery pipe; and

[0010] The membrane assembly has a feed port connected to the other end of the delivery pipe, a retained liquid outlet connected to the material tank, and the pump can pump the liquid medicine in the material tank into the membrane assembly when it is turned on.

[0011] Preferably, the retentate outlet of the membrane module is connected to a discharge pipe, the discharge pipe is provided with a discharge port, and the discharge pipe and the material tank are connected through a reflux pipe.

[0012] Preferably, a temperature regulating component is provided on the delivery pipe, and the temperature regulating component is used to regulate the temperature of the medicine liquid in the delivery pipe.

[0013] Preferably, a plurality of the membrane modules are provided, and the plurality of the membrane modules are connected to one of the delivery pipes and one of the discharge pipes.

[0014] Preferably, the filter screen is placed on the bottom surface of the material tank and can cover the discharge port.

[0015] Preferably, the membrane assembly is detachable.

[0016] The present invention also provides a method for rapidly separating small molecule compounds in Chinese medicinal materials, using the device for rapidly separating small molecule compounds in Chinese medicinal materials as described above; the steps are as follows:

[0017] Step 1, placing medicinal materials and solvent in the material tank;

[0018] Step 2: Turn on the device switch to start the extraction and membrane treatment process.

[0019] Preferably, the retentate outlet of the membrane assembly is connected to a discharge pipe, the end of the discharge pipe is a discharge port, and the discharge pipe and the material tank are connected through a reflux pipe; in step two, during membrane treatment, the discharge port is closed and the material tank and the discharge pipe are connected; and step three is also included: after the set time of membrane treatment, the discharge port is opened, and the connection between the material tank and the discharge pipe is disconnected, and the retentate discharged from the discharge port is collected.

[0020] Preferably, the medicinal material in step 1 is a bagged powder or granular medicinal material.

[0021] Preferably, the method further comprises step 4: collecting the permeate and concentrating the permeate, and then freeze-drying the permeate into powder or spray-drying the powder to obtain the product.

[0022] Compared with the prior art, the present invention has achieved the following technical effects:

[0023] The device provided by the present invention couples the two steps of extraction and separation in the traditional process, and integrates the extraction process and the membrane separation process in one device, which greatly reduces the production cost and operation difficulty and improves the production efficiency. In addition, the drug solution circulates in the circulation loop of the device to realize multiple extractions and separations to fully extract the small molecule compounds therein and avoid their waste. The use of a cyclic extraction method can weaken the concentration polarization phenomenon of the membrane component. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings required for use in the embodiments will be briefly introduced below. Obviously, the drawings described below are only some embodiments of the present invention. For ordinary technicians in this field, other drawings can be obtained based on these drawings without paying creative work.

[0025] Figure 1 This is a structural block diagram of a device for rapidly separating small molecule compounds in traditional Chinese medicine provided in one embodiment of the present invention.

[0026] Figure 2 for Figure 1 Schematic diagram of the structure of the middle filter.

[0027] Figure 3 Schematic diagram of the changes in membrane flux of the membrane module when the effective ingredients in fenugreek seeds are extracted by the post-extraction membrane method.

[0028] Figure 4 The present invention is a schematic diagram of changes in membrane flux of a membrane assembly when the device provided by the present invention is used to perform coupled extraction and separation on fenugreek seeds.

[0029] Figure 5 For Figure 4 Schematic diagram of the change in membrane flux when the membrane assembly is cleaned.

[0030] Figure 6 Schematic diagram of the comparison of DPPH radical scavenging activity in products obtained from fenugreek seeds extracted using different methods.

[0031] Figure 7 Schematic diagram of the comparison of ABTS+ free radical scavenging activity in products obtained from fenugreek seeds extracted using different methods.

[0032] Figure 8 The present invention is used to extract effective ingredients from water-extracted Gastrodia elata using the device and method provided by the present invention, and a schematic diagram of changes in the membrane flux of the membrane assembly during the extraction process.

[0033] In the figure: 1- material tank; 2- filter screen; 3- temperature regulating component; 4- membrane component; 5- permeate outlet; 6- discharge port; 7- reflux pipe; 8- pump; 9- delivery pipe. DETAILED DESCRIPTION

[0034] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only 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.

[0035] In order to make the above-mentioned objects, features and advantages of the present invention more obvious and easy to understand, the present invention is further described in detail below with reference to the accompanying drawings and specific embodiments.

[0036] First, some technical terms involved in the embodiments of the present application are introduced.

[0037] Concentration polarization refers to the accumulation of solutes (ions or solutes of different molecular weights) on the membrane surface during membrane separation, resulting in a higher solute concentration on the membrane surface than in the bulk solution. This phenomenon can lead to a decrease in the flux of the solvent through the membrane.

[0038] The present invention provides a device for rapidly separating small molecular compounds in Chinese medicinal materials, such as Figure 1-2 As shown, it includes: a material tank 1, a filter screen 2, a delivery pipe 9 and a membrane assembly 4.

[0039] The material tank 1 is used to contain medicinal materials and solvents. A discharge port is provided at the bottom of the material tank 1. The medicinal materials are generally bagged powder or granular medicinal materials to facilitate the precipitation of effective ingredients therein. The components in the medicinal materials are precipitated into the solvent to form a medicinal liquid, and the medicinal liquid is discharged from the discharge port to the next link. The next link in the present invention refers to the temperature adjustment link or the extraction link.

[0040] The filter screen 2 is disposed above the discharge port, and the filter screen 2 is used to prevent the medicinal material particles or medicinal material bags from being discharged from the discharge port. In other words, the filter screen 2 is used to intercept the medicinal material particles or medicinal material bags to the end of the material tank 1.

[0041] One end of the delivery pipe 9 is connected to the discharge port of the material tank 1 , and a pump 8 is provided on the delivery pipe 9 .

[0042] The feed port of the membrane assembly 4 is connected to the other end of the delivery pipe 9. The membrane assembly 4 has a permeate outlet 5 and a retentate outlet. The retentate outlet of the membrane assembly 4 is connected to the material tank 1. Specifically, a discharge pipe can be connected to the retentate outlet of the membrane assembly 4. The discharge pipe is provided with a discharge port 6. The discharge pipe and the material tank 1 are connected through a reflux pipe 7. When the pump 8 is turned on, the liquid medicine in the material tank 1 can be pumped into the membrane assembly 4. The material tank 1, the delivery pipe 9, and the membrane assembly 4 are sequentially connected and connected to form a circulation loop, so as to facilitate multiple extractions and separations of the medicinal materials.

[0043] The device provided by the present invention couples the two steps of extraction and separation in the traditional process, and integrates the extraction process and the membrane separation process into one device, which greatly reduces the production cost and operation difficulty and improves the production efficiency. In addition, the drug solution circulates in the circulation loop of the device to realize multiple extractions and separations to fully extract the small molecule compounds therein and avoid their waste. The use of a cyclic extraction method can weaken the concentration polarization phenomenon of the membrane component 4.

[0044] Principle of reducing concentration polarization phenomenon of membrane module 4:

[0045] When the device of the present invention is used for extraction and separation, the small molecule compounds in the medicinal materials dissolve quickly and pass through the membrane assembly 4 and are collected within a short time after entering the extract. It is difficult for small molecule compounds to accumulate on the membrane surface to form a concentration polarization layer. The macromolecules dissolve slowly, and only a small amount is dissolved in a limited extraction and separation time. Therefore, the thickness of the concentration polarization layer is reduced, which indirectly affects the membrane adsorption and the subsequent membrane contamination degree, so that the membrane contamination is reduced.

[0046] In some embodiments, a temperature regulating component 3 is provided on the delivery tube 9 , and the temperature regulating component 3 is used to regulate the temperature of the drug solution in the delivery tube 9 .

[0047] In some embodiments, a plurality of membrane modules 4 are provided, and the plurality of membrane modules 4 are connected to a delivery pipe 9 and a discharge pipe.

[0048] In this embodiment, the separation efficiency can be adjusted by adjusting the number of membrane modules 4 .

[0049] In some embodiments, the filter screen 2 is placed on the bottom surface of the material tank 1 and can cover the discharge port. The filter screen 2 can also be called a sieve plate.

[0050] In this embodiment, the filter screen 2 is used to place medicinal materials, and the filter screen 2 plays a supporting and intercepting role for the medicinal materials.

[0051] In some embodiments, the membrane assembly 4 is detachable.

[0052] This embodiment facilitates timely replacement of a failed membrane assembly 4 .

[0053] The pipeline of the present invention is provided with a plurality of on-off valves, such as Figure 1 shown.

[0054] The present invention also provides a method for rapidly separating small molecule compounds in Chinese medicinal materials, using the device for rapidly separating small molecule compounds in Chinese medicinal materials as described in the above embodiment; the steps are as follows:

[0055] Step 1: Place medicinal materials and solvent in material tank 1;

[0056] Step 2: Turn on the device switch to start the extraction and membrane treatment process.

[0057] This embodiment has all the advantages of the above-mentioned device for rapidly separating small molecule compounds in Chinese medicinal materials, and will not be described in detail here.

[0058] In some embodiments, the retentate outlet of the membrane assembly 4 is connected to a discharge pipe, the end of the discharge pipe is a discharge port 6, and the discharge pipe and the material tank 1 are connected through a reflux pipe 7; in step two, during the membrane treatment, the discharge port 6 is closed and the material tank 1 and the discharge pipe are connected; it also includes step three: after the set time of membrane treatment, the discharge port 6 is opened, and the connection between the material tank 1 and the discharge pipe is disconnected, and the retentate discharged from the discharge port 6 is collected.

[0059] In some embodiments, the medicinal material in step 1 is a bagged powder or granular medicinal material.

[0060] In some embodiments, the method further comprises step 4: collecting the permeate and concentrating the permeate, and then freeze-drying or spray-drying the permeate into a powder to obtain the product.

[0061] The present invention provides an embodiment using fenugreek seeds as a medicinal material and an ethanol solution as an extract, and the process steps are as follows:

[0062] 1. Crush the fenugreek seeds, weigh 500g of powder and put it evenly into 2 Chinese medicine bags, and tie the bags tightly;

[0063] 2. Place the sieve plate at the bottom of tank 1, then put the medicine bag in, and add 15L 50% ethanol solution;

[0064] 3. Turn on the device switch, keep the pressure at 0.01 kPa, turn on the temperature adjustment component 3, and maintain the temperature at 25°C;

[0065] 4. Open the switch of the permeate outlet 5 to collect the permeate;

[0066] 5. After 45 minutes of extraction, add 10L 50% ethanol solution for top washing;

[0067] 6. After 1.5 hours of extraction, turn off the device, open the retentate outlet switch, and collect the retentate;

[0068] 7. After the permeate is concentrated, freeze-dried into powder to obtain the product.

[0069] In order to better reflect the advantages of the device and method for quickly separating small molecule compounds in Chinese medicinal materials provided by the present invention, the inventor used fenugreek seeds as medicinal materials for extraction and conducted several tests. The first type of coupled extraction is to use the device and method for quickly separating small molecule compounds in Chinese medicinal materials provided by the present invention to couple the components in the medicinal materials. The second type is the traditional solvent extraction method, and the third type is to use the extraction equipment alone to extract the medicinal materials and then separate them through a membrane.

[0070] The results of the products obtained by extraction are shown in the following table.

[0071] Table 1 Comparison of coupled extraction with traditional solvent extraction and extraction followed by membrane extraction - extraction rate (mg / g medicinal material)

[0072]

[0073] Table 2 Comparison of coupled extraction with traditional solvent extraction and extraction followed by membrane extraction - Extract purity (%)

[0074]

[0075] It can be seen from the above two tables that the extraction rate of secondary metabolites obtained by the coupled extraction method is basically equivalent to or higher than that of the traditional solvent extraction method and the membrane method after extraction, and the purity of the extract has been greatly improved compared with the traditional method.

[0076] like Figure 3 Schematic diagram of the change in membrane flux of the membrane module when the third type of extraction and subsequent membrane separation is adopted.

[0077] like Figure 4 The diagram is a schematic diagram of changes in membrane flux of a membrane assembly when the equipment provided by the present invention is used to perform coupled extraction and separation on fenugreek seeds.

[0078] like Figure 5 For Figure 4 Schematic diagram of the change in membrane flux when the membrane assembly is cleaned.

[0079] Figure 6 This is a schematic diagram comparing the DPPH free radical scavenging activity in products obtained by different methods, with ascorbic acid (VC) with strong antioxidant activity as a positive control.

[0080] Figure 7 Schematic diagram for comparison of ABTS+ free radical scavenging activity in products obtained by different methods, with ascorbic acid (VC) having strong antioxidant activity as a positive control.

[0081] The inventors also used the device and method provided by the present invention to extract the effective components from water-extracted Gastrodia elata. The schematic diagram of the change of the membrane flux of the membrane assembly during the extraction process is shown in FIG. Figure 8 shown.

[0082] The results of the products obtained by extraction are shown in the following table.

[0083] Table 1 Comparison of coupled extraction with traditional solvent extraction and extraction followed by membrane extraction - extraction rate (mg / g medicinal material)

[0084]

[0085] Table 2 Comparison of coupled extraction with traditional solvent extraction and extraction followed by membrane purification - Purity (%)

[0086]

[0087] As shown in Table 1 and Table 2, the extraction rate and purity of the effective components extracted from Gastrodia elata by this process are higher than those by the traditional method. Therefore, the coupled extraction process is expected to be applied to the separation and purification of various traditional Chinese medicine products.

[0088] The present invention uses specific examples to illustrate the principles and implementation methods of the present invention. The above examples are only used to help understand the method and core ideas of the present invention. At the same time, for those skilled in the art, according to the ideas of the present invention, there will be changes in the specific implementation methods and application scope. In summary, the content of this specification should not be understood as limiting the present invention.

Claims

1. A device for rapidly separating small molecular compounds in Chinese medicinal materials, characterized in that: include: A material tank, used to contain medicinal materials and solvents, with a discharge port provided at the bottom of the material tank; A filter screen, wherein the filter screen cover is arranged above the discharge port; A delivery pipe, one end of which is connected to the discharge port of the material tank, and a pump is provided on the delivery pipe; as well as The membrane assembly has a feed port connected to the other end of the delivery pipe, a retained liquid outlet connected to the material tank, and the pump can pump the liquid medicine in the material tank into the membrane assembly when it is turned on.

2. The device for rapidly separating small molecule compounds in Chinese medicinal materials according to claim 1, characterized in that: The retentate outlet of the membrane module is connected to a discharge pipe, a discharge port is arranged on the discharge pipe, and the discharge pipe is connected to the material tank through a reflux pipe.

3. The device for rapidly separating small molecule compounds in Chinese medicinal materials according to claim 1, characterized in that: The delivery pipe is provided with a temperature regulating component, and the temperature regulating component is used to regulate the temperature of the medicine liquid in the delivery pipe.

4. The device for rapidly separating small molecule compounds in Chinese medicinal materials according to claim 2, characterized in that: A plurality of the membrane modules are provided, and the plurality of the membrane modules are connected with one of the transport pipes and one of the discharge pipes.

5. The device for rapid separation of small molecule compounds in Chinese medicinal materials according to claim 1, characterized in that: The filter screen is placed on the bottom surface of the material tank and can cover the discharge port.

6. The device for rapid separation of small molecule compounds in Chinese medicinal materials according to claim 1, characterized in that: The membrane assembly is detachable.

7. A method for rapidly separating small molecule compounds in Chinese medicinal materials, characterized in that: The device for rapidly separating small molecule compounds in Chinese medicinal materials according to any one of claims 1 to 6 is used; the steps are as follows: Step 1, placing medicinal materials and solvent in the material tank; Step 2: Turn on the device switch to start the extraction and membrane treatment process.

8. The method for rapid separation of small molecule compounds in Chinese medicinal materials according to claim 7, characterized in that: The retentate outlet of the membrane assembly is connected to a discharge pipe, the end of the discharge pipe is a discharge port, and the discharge pipe and the material tank are connected through a reflux pipe; in step two, during the membrane treatment, the discharge port is closed and the material tank and the discharge pipe are connected; and step three is also included: after the set time of membrane treatment, the discharge port is opened, and the connection between the material tank and the discharge pipe is disconnected, and the retentate discharged from the discharge port is collected.

9. The method for rapid separation of small molecule compounds in Chinese medicinal materials according to claim 8, characterized in that: The medicinal materials in step 1 are powdered or granular medicinal materials in bags.

10. The method for rapid separation of small molecule compounds in Chinese medicinal materials according to claim 9, characterized in that: The method also includes step 4: collecting the permeate and concentrating the permeate, and then freeze-drying or spray-drying the permeate into powder to obtain the product.

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