Membrane extraction process for effective components in traditional Chinese medicine liquid
By performing microfiltration, ultrafiltration, nanofiltration in an additional electric field and combining molecular imprinting technology, the problem of loss of effective ingredients and low purity of traditional Chinese medicine liquid refining is solved, and efficient traditional Chinese medicine liquid refining is achieved, which significantly improves the Purity and recovery of ingredients.
Patent Information
- Application Number
- CN202411514590.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-29
- Publication Date
- 2024-12-13
AI Technical Summary
Existing methods for refining traditional Chinese medicine liquids such as alcohol precipitation method, flocculation clarification method and macroporous resin method have problems such as loss of drug-effective ingredients, insufficient refining degree, low safety and purity indicators, and the residual problems of chemical separation media are difficult to solve.
Pretreatment of traditional Chinese medicine liquid by microfiltration, ultrafiltration and nanofiltration in an additional electric field, and extracting active ingredients through molecular blotting technology. Separation of microfiltration membrane, ultrafiltration membrane and nanofiltration membrane are used. The voltage between the cathode is 0.1~1kv, and the high-speed centrifuge is performed by a disc centrifuge.
It significantly improves the purity and recovery rate of the active ingredients, slows down membrane pollution, accelerates filtration efficiency, and ensures efficient refining of traditional Chinese medicine liquids.
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Figure CN119113803A_ABST
Abstract
Description
Technical Field
[0001] The invention relates to the technical field of extraction of effective components of traditional Chinese medicine, and in particular to a membrane extraction process of effective components in traditional Chinese medicine liquid. Background Art
[0002] The methods commonly used to purify Chinese herbal medicine extracts mainly include alcohol precipitation, flocculation clarification and macroporous resin adsorption, etc., all of which aim to remove non-drug-effective high-molecular substances. The main technical principle of the alcohol precipitation method is to use the different solubility of large and small molecular substances in ethanol to form precipitation and remove high-molecular substances; the flocculation clarification method is to remove coarse particles in the solution by adding clarifiers to adsorb bridging and charge neutralization; the macroporous adsorption resin method is to use the difference in the sieving porosity and van der Waals force of macroporous resins for different molecules to separate substances.
[0003] The above methods can achieve different degrees of purification effects, but they all have common problems such as loss of active ingredients and low degree of purification, and they also have their own defects. For example, the alcohol precipitation method takes a long time, is costly, and has adverse effects on subsequent processes and clinical efficacy; the flocculation method and macroporous resin method use chemical separation media, which have problems with flocculants or resin residues. In short, the above purification technologies are not satisfactory in terms of safety, effectiveness and purity indicators. Summary of the invention
[0004] To solve the above problems, the present invention provides a membrane extraction process for active ingredients in traditional Chinese medicine liquid, which pretreats the traditional Chinese medicine liquid by microfiltration, ultrafiltration and nanofiltration in an additional electric field, and uses synergistic molecular imprinting technology to significantly improve the purity of the active ingredients.
[0005] To achieve the above object, the technical solution adopted by the present invention is:
[0006] A membrane extraction process for active ingredients in a traditional Chinese medicine liquid comprises the following steps: in an additional electric field, a microfiltration membrane and / or an ultrafiltration membrane and / or a nanofiltration membrane are used to process the traditional Chinese medicine liquid, and the active ingredients are extracted by molecular imprinting technology.
[0007] Furthermore, in the additional electric field, the voltage between the anode and the cathode is 0.1 to 1 kV, the anode is placed on the water inlet side of the microfiltration membrane and / or ultrafiltration membrane and / or nanofiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane and / or ultrafiltration membrane and / or nanofiltration membrane.
[0008] Furthermore, each microfiltration membrane and / or ultrafiltration membrane and / or nanofiltration membrane is configured with at least one pair of anode and cathode.
[0009] Furthermore, the membrane extraction process of the effective ingredients in the traditional Chinese medicine liquid described in the present invention comprises the following steps:
[0010] S1. Centrifuge the Chinese medicine liquid at high speed for 20 to 30 minutes using a disc centrifuge to obtain a centrifuge;
[0011] S2, in an additional electric field, microfiltration separation of the obtained centrifuge liquid to obtain a microfiltration separation liquid;
[0012] S3, in an additional electric field, ultrafiltration separation of the obtained microfiltration separation liquid to obtain an ultrafiltration separation liquid;
[0013] S4, in an additional electric field, performing nanofiltration separation on the obtained ultrafiltration separation liquid to obtain a nanofiltration separation liquid;
[0014] S5. In an additional electric field, the effective components in the nanofiltration separation liquid are extracted by molecular imprinting technology.
[0015] Furthermore, in the step S1, the rotation speed of the high-speed centrifugation is 7000-8000 r / min.
[0016] Furthermore, in the step S2, a ceramic membrane with a pore size of 0.05 to 0.1 μm and a membrane material of Al2O3 is selected.
[0017] Furthermore, in the step S3, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is selected.
[0018] Furthermore, in the step S4, a nanofiltration membrane with a molecular weight cutoff of 150 to 300 and a membrane material of polyamide is used.
[0019] The present invention has the following beneficial effects:
[0020] Pretreatment of Chinese herbal medicine by microfiltration, ultrafiltration and nanofiltration in an additional electric field can increase filtration efficiency and reduce membrane pollution; the use of molecular imprinting technology in an additional electric field can significantly improve the purity of the active ingredients. BRIEF DESCRIPTION OF THE DRAWINGS
[0021] Other features, objects and advantages of the present invention will become more apparent from the detailed description of non-limiting embodiments made with reference to the following drawings:
[0022] Figure 1 Figure 2 is a graph showing the microfiltration completion time for each group.
[0023] Figure 2 The graph shows the ultrafiltration completion time of each group.
[0024] Figure 3 Figure 2 is a graph showing the nanofiltration completion time of each group.
[0025] Figure 4 is the recovery and extraction rate of baicalin in each group.
[0026] Figure 5 is the purity of baicalin in each group. DETAILED DESCRIPTION
[0027] The present invention is described in detail below in conjunction with specific embodiments. The following embodiments will help those skilled in the art to further understand the present invention, but are not intended to limit the present invention in any form. It should be noted that, for those of ordinary skill in the art, several variations and improvements may be made without departing from the concept of the present invention. These all belong to the protection scope of the present invention.
[0028] In the following embodiments:
[0029] The molecularly imprinted polymer is prepared by using the target molecule as the template molecule, methacrylic acid (MAA) as the functional monomer, ethylene glycol dimethacrylate (EDMA) as the crosslinking agent, azobisisobutyronitrile as the initiator, and acetonitrile as the porogen. The molar ratio of the template molecule, the functional monomer, the crosslinking agent, the porogen and the initiator is 1:4:20:40:0.1. The preparation method refers to the existing patent CN201310469622.4. In Examples 1-3, baicalein is used as the template molecule, and in Example 4, matrine is used as the template molecule.
[0030] Example 1
[0031] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0032] S1. Centrifuge the Radix Scutellariae Radix (prepared by hot reflux extraction) at high speed for 30 min in a disc centrifuge at a speed of 7000 r / min to obtain a centrifuge;
[0033] S2. In the additional electric field, a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 is used to separate the centrifuge liquid by microfiltration, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0034] S3. In an additional electric field, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is used to ultrafiltration separate the obtained microfiltration separated liquid. The ultrafiltration temperature is 35° C. and the membrane pressure is 8 bar to obtain an ultrafiltration separated liquid.
[0035] S4. In an additional electric field, the ultrafiltration separation liquid is separated by nanofiltration using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide. The nanofiltration temperature is 50° C. and the operating pressure is 10 bar to obtain a retentate.
[0036] S5. In an additional electric field, a molecular imprinting polymer with baicalein as a template molecule is used to extract baicalein from the retentate.
[0037] In the additional electric field of this embodiment, each microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane is configured with a pair of anodes and cathodes. The anode is placed on the water inlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane. The voltage between the anode and the cathode is 0.1kV.
[0038] Example 2
[0039] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0040] S1. Centrifuge the Radix Scutellariae Radix (prepared by hot reflux extraction) at high speed for 20 min in a disc centrifuge at a speed of 8000 r / min to obtain a centrifuge;
[0041] S2. In the additional electric field, a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 is used to separate the centrifuge liquid by microfiltration, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0042] S3. In an additional electric field, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is used to ultrafiltration separate the obtained microfiltration separated liquid. The ultrafiltration temperature is 35° C. and the membrane pressure is 8 bar to obtain an ultrafiltration separated liquid.
[0043] S4. In an additional electric field, the ultrafiltration separation liquid is separated by nanofiltration using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide. The nanofiltration temperature is 50° C. and the operating pressure is 10 bar to obtain a retentate.
[0044] S5. In an additional electric field, a molecular imprinting polymer with baicalein as a template molecule is used to extract baicalein from the retentate.
[0045] In the additional electric field of this embodiment, each microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane is configured with a pair of anodes and cathodes. The anode is placed on the water inlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane. The voltage between the anode and the cathode is 0.5kV.
[0046] Example 3
[0047] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0048] S1. Centrifuge the Radix Scutellariae Radix (prepared by hot reflux extraction) at high speed for 25 min in a disc centrifuge at a speed of 7500 r / min to obtain a centrifuge;
[0049] S2. In the additional electric field, a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 is used to separate the centrifuge liquid by microfiltration, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0050] S3. In an additional electric field, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is used to ultrafiltration separate the obtained microfiltration separated liquid. The ultrafiltration temperature is 35° C. and the membrane pressure is 8 bar to obtain an ultrafiltration separated liquid.
[0051] S4. In an additional electric field, the ultrafiltration separation liquid is separated by nanofiltration using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide. The nanofiltration temperature is 50° C. and the operating pressure is 10 bar to obtain a retentate.
[0052] S5. In an additional electric field, a molecular imprinting polymer with baicalein as a template molecule is used to extract baicalein from the retentate.
[0053] In the additional electric field of this embodiment, each microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane is configured with a pair of anodes and cathodes. The anode is placed on the water inlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane. The voltage between the anode and the cathode is 1 kV.
[0054] Example 4
[0055] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0056] S1. Centrifuge the Radix Sophorae Flavescentis liquid (prepared by hot reflux extraction method) at high speed for 25 min in a disc centrifuge at a speed of 7500 r / min to obtain a centrifuge;
[0057] S2. In the additional electric field, a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 is used to separate the centrifuge liquid by microfiltration, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0058] S3. In an additional electric field, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is used to ultrafiltration separate the obtained microfiltration separated liquid. The ultrafiltration temperature is 35° C. and the membrane pressure is 8 bar to obtain an ultrafiltration separated liquid.
[0059] S4. In an additional electric field, the ultrafiltration separation liquid is separated by nanofiltration using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide. The nanofiltration temperature is 50° C. and the operating pressure is 10 bar to obtain a retentate.
[0060] S5. In an additional electric field, a molecular imprinting polymer using matrine as a template molecule is used to extract matrine from the retentate.
[0061] In the additional electric field of this embodiment, each microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane is configured with a pair of anodes and cathodes. The anode is placed on the water inlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane. The voltage between the anode and the cathode is 0.5kV.
[0062] Comparative Example 1
[0063] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0064] S1. Centrifuge the Radix Scutellariae Radix (prepared by hot reflux extraction) at high speed for 25 min in a disc centrifuge at a speed of 7500 r / min to obtain a centrifuge;
[0065] S2, using a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 to separate the centrifuge liquid, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0066] S3. In an additional electric field, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is used to ultrafiltration separate the obtained microfiltration separated liquid. The ultrafiltration temperature is 35° C. and the membrane pressure is 8 bar to obtain an ultrafiltration separated liquid.
[0067] S4. In an additional electric field, the ultrafiltration separation liquid is separated by nanofiltration using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide. The nanofiltration temperature is 50° C. and the operating pressure is 10 bar to obtain a retentate.
[0068] S5. In an additional electric field, a molecular imprinting polymer with baicalein as a template molecule is used to extract baicalein from the retentate.
[0069] In the additional electric field of this embodiment, each ultrafiltration membrane and nanofiltration membrane is configured with a pair of anode and cathode, the anode is placed on the water inlet side of the ultrafiltration membrane and nanofiltration membrane, and the cathode is placed on the water outlet side of the ultrafiltration membrane and nanofiltration membrane, and the voltage between the anode and the cathode is 1kV.
[0070] Comparative Example 2
[0071] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0072] S1. Centrifuge the Radix Scutellariae Radix (prepared by hot reflux extraction) at high speed for 25 min in a disc centrifuge at a speed of 7500 r / min to obtain a centrifuge;
[0073] S2. In the additional electric field, a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 is used to separate the centrifuge liquid by microfiltration, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0074] S3, using an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 to perform ultrafiltration separation on the obtained microfiltration separation liquid, at an ultrafiltration temperature of 35°C and a membrane outlet pressure of 8 bar, to obtain an ultrafiltration separation liquid;
[0075] S4. In an additional electric field, the ultrafiltration separation liquid is separated by nanofiltration using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide. The nanofiltration temperature is 50° C. and the operating pressure is 10 bar to obtain a retentate.
[0076] S5. In an additional electric field, a molecular imprinting polymer with baicalein as a template molecule is used to extract baicalein from the retentate.
[0077] In the additional electric field of this embodiment, each microfiltration membrane and nanofiltration membrane is configured with a pair of anode and cathode, the anode is placed on the water inlet side of the microfiltration membrane and nanofiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane and nanofiltration membrane. The voltage between the anode and the cathode is 1kV.
[0078] Comparative Example 3
[0079] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0080] S1. Centrifuge the Radix Scutellariae Radix (prepared by hot reflux extraction) at high speed for 25 min in a disc centrifuge at a speed of 7500 r / min to obtain a centrifuge;
[0081] S2. In the additional electric field, a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 is used to separate the centrifuge liquid by microfiltration, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0082] S3. In an additional electric field, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is used to ultrafiltration separate the obtained microfiltration separated liquid. The ultrafiltration temperature is 35° C. and the membrane pressure is 8 bar to obtain an ultrafiltration separated liquid.
[0083] S4, using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide to separate the obtained ultrafiltration separation liquid, the nanofiltration temperature is 50° C., the operating pressure is 10 bar, and a retentate is obtained;
[0084] S5. In an additional electric field, a molecular imprinting polymer with baicalein as a template molecule is used to extract baicalein from the retentate.
[0085] In the additional electric field of this embodiment, each microfiltration membrane and ultrafiltration membrane is configured with a pair of anode and cathode, the anode is placed on the water inlet side of the microfiltration membrane and ultrafiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane and ultrafiltration membrane. The voltage between the anode and the cathode is 1kV.
[0086] Comparative Example 4
[0087] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0088] S1. Centrifuge the Radix Scutellariae Radix (prepared by hot reflux extraction) at high speed for 25 min in a disc centrifuge at a speed of 7500 r / min to obtain a centrifuge;
[0089] S2. In the additional electric field, a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 is used to separate the centrifuge liquid by microfiltration, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0090] S3. In an additional electric field, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is used to ultrafiltration separate the obtained microfiltration separated liquid. The ultrafiltration temperature is 35° C. and the membrane pressure is 8 bar to obtain an ultrafiltration separated liquid.
[0091] S4. In an additional electric field, the ultrafiltration separation liquid is separated by nanofiltration using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide. The nanofiltration temperature is 50° C. and the operating pressure is 10 bar to obtain a retentate.
[0092] S5. The extraction of baicalin from the retentate is achieved by using a molecular imprinting polymer with baicalin as a template molecule.
[0093] In the additional electric field of this embodiment, each microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane is configured with a pair of anodes and cathodes. The anode is placed on the water inlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane. The voltage between the anode and the cathode is 1 kV.
[0094] Comparative Example 5
[0095] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0096] S1. Centrifuge the Radix Scutellariae Radix (prepared by hot reflux extraction) at high speed for 25 min in a disc centrifuge at a speed of 7500 r / min to obtain a centrifuge;
[0097] S2, using a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 to separate the centrifuge liquid, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0098] S3, using an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 to perform ultrafiltration separation on the obtained microfiltration separation liquid, at an ultrafiltration temperature of 35°C and a membrane outlet pressure of 8 bar, to obtain an ultrafiltration separation liquid;
[0099] S4, using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide to separate the obtained ultrafiltration separation liquid, the nanofiltration temperature is 50° C., the operating pressure is 10 bar, and a retentate is obtained;
[0100] S5. The extraction of baicalin from the retentate is achieved by using a molecular imprinting polymer with baicalin as a template molecule.
[0101] Comparative Example 6
[0102] A membrane extraction process for effective ingredients in a traditional Chinese medicine liquid comprises the following steps:
[0103] S1. Centrifuge the Radix Sophorae Flavescentis liquid (prepared by hot reflux extraction method) at high speed for 25 min in a disc centrifuge at a speed of 7500 r / min to obtain a centrifuge;
[0104] S2, using a ceramic membrane with a pore size of 0.05 μm and a membrane material of AL2O3 to separate the centrifuge liquid, with an operating temperature of 45°C and a membrane outlet pressure of 1.0 bar to obtain a microfiltration separation liquid;
[0105] S3, using an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 to perform ultrafiltration separation on the obtained microfiltration separation liquid, at an ultrafiltration temperature of 35°C and a membrane outlet pressure of 8 bar, to obtain an ultrafiltration separation liquid;
[0106] S4, using a nanofiltration membrane with a molecular weight cutoff of 200 and a membrane material of polyamide to separate the obtained ultrafiltration separation liquid, the nanofiltration temperature is 50° C., the operating pressure is 10 bar, and a retentate is obtained;
[0107] S5. The extraction of matrine from the retentate is achieved by using a molecular imprinting polymer with matrine as a template molecule.
[0108] Test data
[0109] The completion time of microfiltration, ultrafiltration and nanofiltration in each group was recorded respectively. The results are shown in Table 1. Figure 1 , Figure 2 and Figure 3 :
[0110] Table 1 Completion schedule of each group of microfiltration, ultrafiltration and nanofiltration
[0111]
[0112]
[0113] From Table 1, we can see that:
[0114] 1) The microfiltration completion time, ultrafiltration completion time, and nanofiltration completion time of Examples 1 to 3 are all shortened as the voltage between the anode and the cathode increases. In order to explore whether this rule exists consistently, the voltage between the anode and the cathode is subsequently adjusted to 1.1 kV and 1.5 kV, respectively. The results show that at 1.1 kV, the microfiltration completion time, ultrafiltration completion time, and nanofiltration completion time are basically the same as those at 1 kV, while at 1.5 kV, the microfiltration completion time, ultrafiltration completion time, and nanofiltration completion time are actually increased compared to 1 kV. Based on this, the voltage range between the anode and the cathode is set to 0.1 to 1 kV.
[0115] 2) Compared with Example 3, the microfiltration completion time of Comparative Example 1 is significantly increased. It can be seen that the design of the additional electric field can significantly shorten the time for microfiltration to complete. The reason may be that the addition of the electric field reduces the membrane resistance of the ceramic membrane and improves the membrane flux. At the same time, since the electric field is not added in the microfiltration stage, the subsequent ultrafiltration time is significantly increased compared with Example 3 although the electric field is added. It can be seen that whether the electric field is added in the microfiltration stage also has an impact on the subsequent ultrafiltration completion time. Similarly, whether the electric field is added in the microfiltration stage also has an impact on the subsequent nanofiltration completion time.
[0116] 3) Compared with Example 3, the ultrafiltration completion time of Comparative Example 2 increased by 18 minutes. It can be seen that the design of the additional electric field can significantly shorten the ultrafiltration completion time. At the same time, in the nanofiltration stage, although the electric field was added, the nanofiltration time was still increased by 10 minutes compared with Example 3. It can be seen that whether the electric field is added in the ultrafiltration stage also has an impact on the subsequent nanofiltration completion time.
[0117] 4) Compared with Example 3, the nanofiltration completion time of Comparative Example 3 was significantly increased. It can be seen that the design of the additional electric field can significantly shorten the nanofiltration completion time.
[0118] 5) Compared with Example 3, the microfiltration completion time, ultrafiltration completion time, and nanofiltration completion time of Comparative Example 5 are significantly increased; at the same time, compared with Example 4, the microfiltration completion time, ultrafiltration completion time, and nanofiltration completion time of Comparative Example 6 are also significantly increased. It can be seen that adding an electric field to microfiltration, ultrafiltration, and nanofiltration can significantly shorten the microfiltration completion time, ultrafiltration completion time, and nanofiltration completion time; at the same time, by comparing Comparative Examples 1-3 and Comparative Example 5, it can be found that whether an electric field is added in microfiltration can affect the subsequent ultrafiltration completion time and nanofiltration completion time, and at the same time, whether an electric field is added in ultrafiltration can affect the subsequent nanofiltration completion time.
[0119] The recovery rate of baicalein in Examples 1-3 and Comparative Examples 1-5 was detected, and the purity of baicalein obtained in Examples 1-3 and Comparative Examples 1-5 was detected by high performance liquid chromatography. The results are shown in Table 2. Figure 4 and Figure 5 .
[0120] Table 2 Baicalin purity of each group
[0121] Group Recovery rate (%) purity(%) Example 1 97.9 98.1 Example 2 98.6 98.7 Example 3 99.7 99.3 Comparative Example 1 95.7 97.1 Comparative Example 2 96.5 97.6 Comparative Example 3 97.6 98.2 Comparative Example 4 99.3 97.9 Comparative Example 5 95.3 96.7
[0122] It can be seen from Table 2 that compared with Example 3, the recovery rate and purity of Comparative Example 1, Comparative Example 2, and Comparative Example 3 are all reduced, and the recovery rate and purity of Comparative Example 5 are the lowest, and the recovery rate and purity decrease rate of Comparative Example 4 are the lowest. It can be seen that there is a synergistic relationship between the operation of the additional electric field when the microfiltration membrane, ultrafiltration membrane, and nanofiltration membrane are used to treat the traditional Chinese medicine liquid and when the effective ingredient is extracted by molecular imprinting technology. The combination of the four can significantly improve the recovery rate and purity of baicalin.
[0123] At the same time, the recovery rate of matrine in Example 4 and Comparative Example 6 was detected, and the purity of matrine obtained in Example 4 and Comparative Example 6 was detected by high performance liquid chromatography. The results showed that compared with Example 4, the recovery rate and purity of Comparative Example 6 were significantly reduced, by 3.9% and 1.6%, respectively. It can be seen that the recovery rate and purity of matrine can be significantly improved by adding an electric field when using microfiltration, ultrafiltration, nanofiltration and molecular imprinting technology.
[0124] The above describes the specific embodiments of the present invention. It should be understood that the present invention is not limited to the above specific embodiments, and those skilled in the art may make various modifications or variations within the scope of the claims, which do not affect the essence of the present invention.
Claims
1. A membrane extraction process for active ingredients in a Chinese medicine solution, characterized in that: In the additional electric field, the Chinese medicine liquid is treated by using a microfiltration membrane and / or an ultrafiltration membrane and / or a nanofiltration membrane, and the effective components are extracted by molecular imprinting technology.
2. The membrane extraction process for active ingredients in a Chinese medicine liquid as claimed in claim 1, characterized in that: In the additional electric field, the voltage between the anode and the cathode is 0.1-1 kV, the anode is placed on the water inlet side of the microfiltration membrane and / or ultrafiltration membrane and / or nanofiltration membrane, and the cathode is placed on the water outlet side of the microfiltration membrane and / or ultrafiltration membrane and / or nanofiltration membrane.
3. The membrane extraction process for active ingredients in a Chinese medicine liquid as claimed in claim 1, characterized in that: Each microfiltration membrane and / or ultrafiltration membrane and / or nanofiltration membrane is equipped with at least one pair of anode and cathode.
4. The membrane extraction process for active ingredients in a Chinese medicine liquid as claimed in claim 1, characterized in that: The steps include: S1. Centrifuge the Chinese medicine liquid at high speed for 20 to 30 minutes using a disc centrifuge to obtain a centrifuge; S2, in an additional electric field, microfiltration separation of the obtained centrifuge liquid to obtain a microfiltration separation liquid; S3, in an additional electric field, ultrafiltration separation of the obtained microfiltration separation liquid to obtain an ultrafiltration separation liquid; S4, in an additional electric field, separating the ultrafiltration separation liquid by nanofiltration to obtain a retentate; S5. In an additional electric field, the effective components in the retentate are extracted by molecular imprinting technology.
5. The membrane extraction process for active ingredients in a Chinese medicine liquid as claimed in claim 4, characterized in that: In the step S1, the rotation speed of the high-speed centrifuge is 7000-8000 r / min.
6. The membrane extraction process for active ingredients in a Chinese medicine liquid as claimed in claim 4, characterized in that: In the step S2, a ceramic membrane with a pore size of 0.05-0.1 μm and a membrane material of Al2O3 is selected.
7. The membrane extraction process for active ingredients in a Chinese medicine liquid as claimed in claim 4, characterized in that: In the step S3, an ultrafiltration membrane made of polyvinylidene fluoride and having a molecular weight cutoff of 50,000 is selected.
8. The membrane extraction process for active ingredients in a Chinese medicine liquid as claimed in claim 4, characterized in that: In the step S4, a nanofiltration membrane with a molecular weight cutoff of 150 to 300 and a membrane material of polyamide is used.
