A method for high-efficiency extraction of matrine based on microwave cooperation and ultrasonic assistance

By optimizing the raw material pretreatment and composite wetting solution system, and combining microwave and ultrasonic synergistic extraction, the problems of low extraction efficiency and low purity of matrine were solved, achieving efficient and low-energy matrine extraction, which is suitable for industrial production.

CN122145465APending Publication Date: 2026-06-05GANSU SHENMEI YOUXIAN BIOTECHNOLOGY CO LTD
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
GANSU SHENMEI YOUXIAN BIOTECHNOLOGY CO LTD
Filing Date
2026-03-02
Publication Date
2026-06-05

AI Technical Summary

Technical Problem

In existing matrine extraction methods, the combination of microwave and ultrasound does not take into account synergistic timing matching, resulting in insufficient disruption of the raw material cell walls, leading to low extraction efficiency, low purity, and high energy consumption.

Method used

By optimizing the raw material pretreatment process, designing a composite wetting solution system, matching the timing of microwave and ultrasound synergy, and combining freeze-thaw treatment, the cell wall is destroyed by the expansion and contraction of ice crystals, the matrix binding is destroyed by the composite wetting solution, and high-efficiency and high-purity extraction is achieved through microwave and ultrasound synergy extraction.

Benefits of technology

It significantly improves the dissolution efficiency and purity of matrine, increasing the extraction rate by more than 30%, achieving a purity of over 95%, reducing energy consumption by 25-30%, and exhibiting good process stability, making it suitable for industrial applications.

✦ Generated by Eureka AI based on patent content.
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Abstract

The application discloses a kind of matrine high-efficiency extraction methods based on microwave cooperation ultrasonic auxiliary, comprising the following steps: S1: Sophora flavescens raw material pretreatment;S2: pre-soaking treatment;S3: microwave cooperation ultrasonic extraction, the mixture after pre-soaking is placed in extraction device, first microwave processing is opened, microwave power 300-400W, frequency 2450MHz, processing 5-8min;Keep microwave open state, synchronous opening ultrasonic processing, ultrasonic power 150-200W, frequency 40-60kHz, microwave and ultrasonic cooperation processing 10-15min;S4: multistage filtration purification, after extraction mixture is filtered first through 200 mesh filter cloth, collect initial filtrate;Then the initial filtrate is filtered by ceramic membrane, collect membrane filtrate;S5: concentration crystallization;S6: separation and drying.The application is by freeze-thaw pretreatment, compound infiltration liquid infiltration and microwave-ultrasonic cooperation extraction combination process, greatly improve the dissolution efficiency of matrine, extraction time is shortened by more than 60% compared with traditional solvent extraction method, and extraction rate is increased by more than 30%.
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Description

Technical Field

[0001] This invention relates to the field of matrine extraction technology, specifically to a highly efficient matrine extraction method based on microwave-assisted ultrasound. Background Technology

[0002] Matrine is an alkaloid extracted from the roots, stems, and leaves of the legume Sophora flavescens. It has various pharmacological activities, including antibacterial, anti-inflammatory, antiviral, and antitumor effects, and has broad application prospects in the fields of medicine, agriculture, and food.

[0003] Currently, the main extraction methods for matrine include solvent extraction, ultrasonic extraction, microwave extraction, and enzymatic hydrolysis. Among them, solvent extraction is simple to operate, but has low extraction efficiency and is time-consuming. Although ultrasonic extraction and microwave extraction can improve extraction efficiency, they still have problems such as insufficient extraction, low purity of matrine, and high energy consumption when used alone.

[0004] In existing technologies, although some studies have attempted to combine microwaves and ultrasound for alkaloid extraction, most of them are simply simultaneous activations without considering the synergistic timing matching of the two, and without targeted pretreatment of the raw material, the cell walls of the raw material are not sufficiently broken during the extraction process, thus limiting the dissolution efficiency of matrine. At the same time, the wetting solutions used in existing extraction methods are mostly single solvents, which cannot effectively destroy the binding effect between matrine and the raw material matrix, further affecting the extraction efficiency and product purity.

[0005] Therefore, developing an extraction method that can achieve efficient synergy between microwave and ultrasound and improve the dissolution efficiency and purity of matrine is of great practical significance. Summary of the Invention

[0006] To address the problems of low extraction efficiency, low purity, and high energy consumption of matrine in existing technologies, this invention provides a highly efficient matrine extraction method based on microwave-assisted ultrasound. By optimizing the raw material pretreatment process, designing a composite wetting solution system, and matching the timing of microwave and ultrasound synergy, this method achieves efficient and high-purity extraction of matrine while reducing extraction energy consumption.

[0007] A highly efficient extraction method for matrine based on microwave-assisted ultrasound includes the following steps: S1: Pretreatment of Sophora flavescens raw materials Select dried Sophora flavescens roots, remove soil, impurities and rotten parts, and pulverize them to 40-60 mesh using a universal pulverizer to obtain Sophora flavescens powder; place the Sophora flavescens powder in a freezing environment of -18~-22℃ for 2-3 hours, take it out and immediately place it in a constant temperature oven of 35-45℃ for 1-1.5 hours to thaw, and repeat the above freezing-thawing operation twice. In this step, the repeated freezing and thawing process can utilize the expansion and contraction of ice crystals to effectively destroy the cell wall structure of the Sophora flavescens raw material, allowing the solvent to penetrate into the raw material more easily during the subsequent extraction process, thereby improving the dissolution efficiency of matrine. S2: Pre-impregnation treatment The pretreated Sophora flavescens powder was mixed with the compound soaking solution at a solid-liquid ratio of 1:15-1:25 (g / mL). The compound soaking solution was prepared by mixing 5-8% ethanol solution and 0.3-0.5 g / L sodium citrate solution at a volume ratio of 9:1. Place the mixture in a constant temperature water bath and stir and soak for 30-40 minutes at 25-30℃ and 150-200r / min. Ethanol in the composite impregnation solution can act as a polar solvent to initially dissolve matrine, while sodium citrate can adjust the pH of the system to a weakly acidic state, thereby disrupting the binding of matrine with pectin, cellulose and other matrices in the raw materials, while also inhibiting the hydrolysis of matrine and improving the stability and dissolution of matrine. S3: Microwave-assisted ultrasonic extraction Transfer the pre-soaked mixture to the microwave-ultrasound synergistic extraction device, turn on the microwave generator, set the microwave power to 300-400W and the frequency to 2450MHz, and microwave the mixture alone for 5-8 minutes. Keep the microwave generator on and simultaneously turn on the ultrasonic generator. Set the ultrasonic power to 150-200W and the frequency to 40-60kHz, and perform microwave and ultrasonic co-processing for 10-15 minutes. During the co-processing, the temperature of the extraction system is controlled at 50-60℃ by the constant temperature jacket of the extraction device; Microwave treatment alone can quickly raise the system temperature, causing the moisture inside the raw material to evaporate rapidly, and the resulting pressure further breaks down the cell walls. Then, ultrasound is turned on simultaneously, and the cavitation effect of ultrasound generates a large number of microbubbles in the solvent. The shock waves generated when the bubbles burst can accelerate the diffusion of matrine into the solvent. At the same time, the thermal effect of microwaves can maintain the system temperature and promote the dissolution of matrine in the solvent, achieving a highly efficient synergy between microwaves and ultrasound, which greatly improves the extraction efficiency. S4: Multi-stage filtration and purification The extracted mixture was first coarsely filtered through a 200-mesh filter cloth to remove undissolved solid impurities, and the initial filtrate was collected. The initial filtrate is then finely filtered through a ceramic membrane filtration device with a membrane pore size of 0.2-0.4 μm and an operating pressure of 0.2-0.3 MPa to remove fine impurities and colloidal particles from the initial filtrate, and the membrane filtrate is collected. Multi-stage filtration can effectively remove impurities from the extract and improve the purity of the subsequent concentrated crystallized product; S5: Concentrated Crystallization Transfer the membrane filtrate to a rotary evaporator, set the vacuum degree to 0.08-0.09 MPa and the temperature to 60-70℃, and concentrate under reduced pressure until the volume of the concentrated liquid is 1 / 5-1 / 4 of the original membrane filtrate volume; Slowly add 3-5 times the volume of acetone to the concentrate while stirring at a speed of 100-150 r / min. After stirring evenly, place the mixture in a refrigerator at 4-8℃ and let it stand for crystallization for 8-12 hours. Acetone, as a poor solvent, can reduce the solubility of matrine in solution, promoting the crystallization of matrine. Low temperature environment can improve crystallization efficiency and crystal purity. S6: Separation and Drying The crystallized mixture was transferred to a high-speed centrifuge, and the speed was set to 4000-5000 r / min and the centrifugation time was 10-15 min. After centrifugation, the bottom precipitate was collected. The precipitate was placed in a vacuum drying oven, and the temperature was set at 50-60℃ and the vacuum degree at 0.07-0.08MPa. It was dried for 3-4 hours to obtain matrine product. Vacuum drying can quickly remove the solvent from the precipitate at a lower temperature, preventing matrine from decomposing due to high temperatures and ensuring product quality.

[0008] Compared with the prior art, the beneficial effects of the present invention are as follows: 1. High extraction efficiency: Through a combination of freezing-thawing pretreatment, composite wetting solution wetting and microwave-ultrasound synergistic extraction, the dissolution efficiency of matrine is greatly improved. The extraction time is shortened by more than 60% compared with the traditional solvent extraction method, and the extraction rate is increased by more than 30%. 2. High product purity: The multi-stage filtration purification process combined with the destruction of impurities by the composite wetting solution results in a final matrine product with a purity of over 95%, which is superior to the product purity obtained by existing ultrasonic or microwave extraction methods alone. 3. Low energy consumption: The synergistic effect of microwave and ultrasound can achieve efficient extraction at lower power and temperature, reducing energy consumption by 25-30% compared to traditional extraction methods; 4. Good process stability: Through precise control of parameters in each step, large-scale production can be achieved, and the product quality is stable, making it suitable for industrial applications. Detailed Implementation Example 1

[0009] A highly efficient extraction method for matrine based on microwave-assisted ultrasound includes the following steps: S1: Pretreatment of Sophora flavescens raw materials Select dried Sophora flavescens roots, remove impurities and pulverize to 50 mesh to obtain Sophora flavescens powder; place the Sophora flavescens powder in a -20℃ freezing environment for 2.5h, take it out and immediately place it in a 40℃ constant temperature environment for 1.2h to thaw, repeat the freezing-thawing operation twice; S2: Pre-impregnation treatment The pretreated Sophora flavescens powder was mixed with the composite soaking solution at a solid-liquid ratio of 1:20 (g / mL). The composite soaking solution was a mixture of 6% ethanol solution and 0.4 g / L sodium citrate solution at a volume ratio of 9:1. After mixing, the mixture was stirred and soaked for 35 min at 28℃ and 180 r / min. S3: Microwave-assisted ultrasonic extraction Place the pre-soaked mixture into the extraction device, turn on the microwave treatment first, microwave power 350W, frequency 2450MHz, treat for 6min; keep the microwave on. Simultaneously start ultrasonic treatment, ultrasonic power 180W, frequency 50kHz, microwave and ultrasonic synergistic treatment for 12min, and control the temperature of the extraction system at 55℃ during the synergistic treatment. S4: Multi-stage filtration and purification The extracted mixture was first filtered through a 200-mesh filter cloth, and the initial filtrate was collected. Then, the initial filtrate was filtered through a ceramic membrane with a pore size of 0.3 μm and an operating pressure of 0.25 MPa, and the membrane filtrate was collected. S5: Concentrated Crystallization The membrane filtrate was placed in a rotary evaporator and concentrated to 1 / 4 of its original volume under a vacuum of 0.085 MPa and a temperature of 65 °C to obtain a concentrated solution. Add 4 times the volume of acetone to the concentrate, stir well, and then let it stand in a 6°C refrigerated environment for 10 hours to crystallize. S6: Separation and Drying The crystallized mixture was centrifuged at 4500 r / min for 12 min, and the precipitate was collected. The precipitate was placed in a vacuum drying oven and dried for 3.5 hours at a temperature of 55℃ and a vacuum degree of 0.075MPa to obtain matrine product.

[0010] This embodiment was implemented in a standardized laboratory environment, namely room temperature 25±2℃ and normal pressure, which is suitable for high-quality Sophora flavescens raw materials with high dryness and impurity content ≤5%, and is suitable for large-scale industrial production scenarios; the parameter settings are balanced, taking into account extraction efficiency, product purity and energy consumption, and pursuing the optimal comprehensive benefits. Example 2

[0011] A highly efficient extraction method for matrine based on microwave-assisted ultrasound includes the following steps: S1: Pretreatment of Sophora flavescens raw materials Select dried Sophora flavescens roots, remove impurities and pulverize to 40 mesh to obtain Sophora flavescens powder; place the Sophora flavescens powder in a -18℃ freezing environment for 3 hours, take it out and immediately place it in a 35℃ constant temperature environment for 1.5 hours to thaw, repeat the freezing-thawing operation twice; S2: Pre-impregnation treatment The pretreated Sophora flavescens powder was mixed with the composite soaking solution at a solid-liquid ratio of 1:15 (g / mL). The composite soaking solution was a mixture of 5% ethanol solution and 0.3 g / L sodium citrate solution at a volume ratio of 9:1. After mixing, the mixture was stirred and soaked for 40 min at 25℃ and 150 r / min. S3: Microwave-assisted ultrasonic extraction The pre-soaked mixture was placed in the extraction device. Microwave treatment was first turned on at a power of 300W and a frequency of 2450MHz for 8 minutes. While keeping the microwave on, ultrasonic treatment was turned on simultaneously at a power of 150W and a frequency of 40kHz. Microwave and ultrasonic treatment were combined for 15 minutes, and the temperature of the extraction system was controlled at 50℃ during the combined treatment. S4: Multi-stage filtration and purification The extracted mixture was first filtered through a 200-mesh filter cloth, and the initial filtrate was collected. Then, the initial filtrate was filtered through a ceramic membrane with a pore size of 0.2 μm and an operating pressure of 0.2 MPa, and the membrane filtrate was collected. S5: Concentrated Crystallization The membrane filtrate was placed in a rotary evaporator and concentrated to 1 / 5 of its original volume under a vacuum of 0.08 MPa and a temperature of 60°C to obtain a concentrated solution. Three times the volume of acetone was added to the concentrated solution, and after stirring evenly, it was placed in a refrigerated environment at 4°C for 12 hours to crystallize. S6: Separation and Drying The crystallized mixture was centrifuged at 4000 r / min for 15 min, and the precipitate was collected. The precipitate was placed in a vacuum drying oven and dried at 50℃ and 0.07 MPa for 4 h to obtain matrine product.

[0012] This embodiment was implemented in a standardized laboratory environment, namely room temperature 25±2℃ and normal pressure, suitable for Sophora flavescens raw materials of poor quality, containing a small amount of impurities and a moisture content of 8-10%, and suitable for mild extraction scenarios; by adopting conservative parameters to ensure extraction stability, namely low power and long extraction time, the problem of insufficient extraction caused by poor raw material characteristics is avoided. Example 3

[0013] A highly efficient extraction method for matrine based on microwave-assisted ultrasound includes the following steps: S1: Pretreatment of Sophora flavescens raw materials Select dried Sophora flavescens roots, remove impurities and pulverize to 60 mesh to obtain Sophora flavescens powder; place the Sophora flavescens powder in a -22℃ freezing environment for 2 hours, take it out and immediately place it in a 45℃ constant temperature environment for 1 hour to thaw, repeat the freezing-thawing operation twice; S2: Pre-impregnation treatment Pre-soaking treatment: The pre-treated Sophora flavescens powder was mixed with the composite soaking solution at a solid-liquid ratio of 1:25 (g / mL). The composite soaking solution was a mixture of 8% ethanol solution and 0.5 g / L sodium citrate solution at a volume ratio of 9:1. After mixing, the mixture was stirred and soaked for 30 min at 30℃ and 200 r / min. S3: Microwave-assisted ultrasonic extraction The pre-soaked mixture was placed in the extraction device. Microwave treatment was first turned on at a power of 400W and a frequency of 2450MHz for 5 minutes. While keeping the microwave on, ultrasonic treatment was simultaneously turned on at a power of 200W and a frequency of 60kHz. Microwave and ultrasonic treatment were combined for 10 minutes, and the temperature of the extraction system was controlled at 60℃ during the combined treatment. S4: Multi-stage filtration and purification The extracted mixture was first filtered through a 200-mesh filter cloth, and the initial filtrate was collected. Then, the initial filtrate was filtered through a ceramic membrane with a pore size of 0.4 μm and an operating pressure of 0.3 MPa, and the membrane filtrate was collected. S5: Concentrated Crystallization The membrane filtrate was placed in a rotary evaporator and concentrated to 1 / 4 of its original volume under a vacuum of 0.09 MPa and a temperature of 70°C to obtain a concentrated solution. Five times the volume of acetone was added to the concentrated solution, and after stirring evenly, it was placed in a refrigerated environment at 8°C for crystallization for 8 hours. S6: Separation and Drying The crystallized mixture was centrifuged at 5000 r / min for 10 min, and the precipitate was collected. The precipitate was placed in a vacuum drying oven and dried at 60℃ and 0.08 MPa for 3 h to obtain matrine product.

[0014] This embodiment was implemented in a standardized laboratory environment, namely room temperature 25±2℃ and normal pressure, which is suitable for high-quality Sophora flavescens raw materials and applicable to efficient and rapid production scenarios. By refining the particle size of the raw materials, increasing the microwave and ultrasonic power, and increasing the amount of solvent, the extraction cycle is shortened to the maximum extent, which can meet the production needs of high capacity. Comparative Example 1: Traditional Solvent Extraction Method

[0015] S1: Select dried Sophora flavescens root, remove impurities, and pulverize to 50 mesh to obtain Sophora flavescens powder; S2: Mix Sophora flavescens powder with 6% ethanol solution at a solid-liquid ratio of 1:20 (g / mL) and extract by stirring at 28℃ and 180r / min for 2h. S3: Filter the extracted mixture through a 200-mesh filter cloth and collect the filtrate; S4: Place the filtrate in a rotary evaporator and concentrate it to 1 / 4 of the original volume under a vacuum of 0.085 MPa and a temperature of 65°C to obtain a concentrated solution; add 4 times the volume of acetone to the concentrated solution, stir well, and then place it in a refrigerated environment at 6°C for 10 hours to crystallize. S5: Centrifuge the crystallized mixture at 4500 r / min for 12 min and collect the precipitate; place the precipitate in a vacuum drying oven and dry it for 3.5 h at 55℃ and 0.075 MPa to obtain matrine product.

[0016] This comparative example was conducted in a standardized laboratory environment consistent with the examples, namely room temperature 25±2℃ and normal pressure, using a traditional solvent extraction process without microwave-ultrasound synergy, freezing-thawing pretreatment, or composite wetting solution, simulating the traditional industrial extraction environment, and was used to compare and verify the significant advantages of the process of the present invention in extraction efficiency and product purity. Comparative Example 2: Ultrasonic Extraction Method Alone

[0017] S1: Select dried Sophora flavescens root, remove impurities, and pulverize to 50 mesh to obtain Sophora flavescens powder; S2: Mix Sophora flavescens powder with 6% ethanol solution at a solid-liquid ratio of 1:20 (g / mL), and stir and soak for 35 min at 28℃ and 180 r / min. S3: Place the mixture in an ultrasonic extraction device, with an ultrasonic power of 180W and a frequency of 50kHz, and extract ultrasonically for 18 minutes at 55℃. S4: Subsequent filtration, concentration, crystallization, separation and drying steps are the same as in Example 1.

[0018] This comparative example was conducted in a standardized laboratory environment, namely room temperature 25±2℃ and normal pressure, retaining only the single method of ultrasonic extraction, while the other conditions were completely consistent with those of Example 1. It was used to specifically verify the necessity of the "microwave-ultrasound synergy" timing control steps of the present invention and to compare the difference in effects between single ultrasonic extraction and synergistic extraction. Comparative Example 3: Microwave-ultrasound synergistic extraction method without freeze-thaw pretreatment

[0019] S1: Select dried Sophora flavescens root, remove impurities, and pulverize to 50 mesh to obtain Sophora flavescens powder; S2: The pre-wetting treatment is the same as in Example 1; S3: Microwave-assisted ultrasound extraction is the same as in Example 1; S4: Subsequent filtration, concentration, crystallization, separation and drying steps are the same as in Example 1.

[0020] This comparative example was conducted in a standardized laboratory environment, namely room temperature 25±2℃ and normal pressure. Only the "freezing-thawing pretreatment" step was removed, and the remaining process parameters were the same as in Example 1. It was used to verify the key role of freezing-thawing pretreatment in destroying the cell wall of Sophora flavescens raw material and improving the dissolution efficiency of matrine. Comparative Example 4: Microwave-Ultrasonic Synergistic Extraction of Single Ethanol Infusion Solution

[0021] S1: The pretreatment of Sophora flavescens raw material is the same as in Example 1; S2: Mix the pretreated Sophora flavescens powder with a 6% volume fraction ethanol solution (single soaking solution) at a solid-liquid ratio of 1:20 (g / mL), and stir and soak for 35 min at 28℃ and 180 r / min. S3: Microwave-assisted ultrasound extraction is the same as in Example 1; S4: Subsequent filtration, concentration, crystallization, separation and drying steps are the same as in Example 1.

[0022] This comparative example was conducted in a standardized laboratory environment, namely room temperature 25±2℃ and normal pressure. Only a single ethanol solution was used to replace the composite impregnation solution of the present invention, and the other conditions were kept consistent with those in Example 1. This was used to verify the advantages of the ethanol-sodium citrate composite impregnation solution in improving the dissolution of matrine and the purity of the product. Experimental Example

[0023] Matrine extraction experiments were conducted according to the methods of Examples 1-3 and Comparative Examples 1-4 described above. Each experiment was performed in parallel three times, and the average value was taken. During the experiment, 5.0g of Sophora flavescens powder was accurately weighed for each experiment; After extraction, the purity and extraction rate of matrine were determined by high performance liquid chromatography (HPLC). HPLC determination conditions: Agilent ZORBAX SB-C18 column (4.6 mm × 250 mm, 5 μm); mobile phase: acetonitrile-0.05 mol / L potassium dihydrogen phosphate solution (volume ratio 30:70); flow rate: 1.0 mL / min; detection wavelength: 220 nm; column temperature: 30 ℃; injection volume: 20 μL.

[0024] Extraction rate calculation method: Extraction rate (%) = (measured mass of matrine product × purity of product) / (total mass of matrine in matrine raw material) × 100%; The total mass of matrine in the raw material of Sophora flavescens was determined by Soxhlet extraction and was 0.32 g / 5.0 g of Sophora flavescens powder.

[0025] The experimental results of each embodiment and comparative example are shown in Table 1 below: Table 1 The experimental results show that the matrine extraction rate and purity of Examples 1-3 are significantly higher than those of Comparative Examples 1-4, and the extraction time is shorter and the unit energy consumption is lower. Among them, Example 1 has the best overall effect, with an extraction rate of 89.2%, a purity of 96.8%, an extraction time of only 53 min, and a unit energy consumption of 0.85 kWh / g matrine.

[0026] Compared with Comparative Example 1, Example 1 showed that the extraction rate was increased by 32.9 percentage points, the purity was increased by 8.3 percentage points, the extraction time was shortened by 56%, and the unit energy consumption was reduced by 32%, indicating that the microwave-ultrasound synergistic extraction process of the present invention has significant advantages over the traditional solvent extraction method.

[0027] Compared with Comparative Example 2, Example 1 showed an increase of 20.5 percentage points in extraction rate, 6.6 percentage points in purity, and a 19% reduction in unit energy consumption. This indicates that the synergistic effect of microwave and ultrasound can more effectively improve the extraction efficiency and purity of matrine compared with ultrasound extraction alone.

[0028] Compared with Comparative Example 3, the extraction rate of Example 1 increased by 13.9 percentage points, indicating that the freeze-thaw pretreatment can effectively destroy the cell wall structure of Matrine raw material and improve the dissolution efficiency of matrine. Compared with Comparative Example 4, the extraction rate of Example 1 increased by 10.6 percentage points and the purity increased by 3 percentage points, indicating that the composite wetting solution can better break the binding between matrine and the raw material matrix, thereby increasing the dissolution amount and purity of matrine. Embodiment 1 of the present invention is the optimal embodiment, and its parameter settings comprehensively consider factors such as extraction efficiency, purity, and energy consumption, making it suitable for large-scale industrial production. The parameter settings in Example 2 are relatively mild and suitable for extraction from Sophora flavescens raw materials of poor quality. Example 3 has the shortest extraction time and is suitable for scenarios with high extraction efficiency requirements; In practical applications, the process parameters of this invention can be appropriately adjusted according to factors such as the quality of the Sophora flavescens raw material and production requirements. For example, when the moisture content of the raw material of Sophora flavescens is high, the microwave treatment time can be appropriately extended; When the purity requirement of matrine is high, the number of ceramic membrane filtration stages can be increased or a ceramic membrane with a smaller pore size can be selected. When it is necessary to improve production efficiency, the microwave and ultrasonic power can be increased appropriately to shorten the extraction time.

Claims

1. A method for efficient extraction of matrine based on microwave-assisted ultrasound, characterized in that, Includes the following steps: S1: Pretreatment of Sophora flavescens raw materials After removing impurities from the dried Sophora flavescens root, it is pulverized to 40-60 mesh to obtain Sophora flavescens powder. The Sophora flavescens powder is pretreated in a freezing environment of -18~-22℃ for 2-3 hours. After taking it out, it is immediately placed in a constant temperature environment of 35-45℃ to thaw for 1-1.5 hours. The freezing-thawing operation is repeated twice. S2: Pre-impregnation treatment The above-mentioned Sophora flavescens powder was mixed with the compound soaking solution at a solid-liquid ratio of 1:15-1:25 (g / mL). The compound soaking solution was a mixture of 5-8% ethanol solution and 0.3-0.5 g / L sodium citrate solution. S3: Microwave-assisted ultrasonic extraction Place the pre-soaked mixture in the extraction device, first turn on the microwave treatment, microwave power 300-400W, frequency 2450MHz, for 5-8 minutes; keep the microwave on and simultaneously turn on the ultrasonic treatment, ultrasonic power 150-200W, frequency 40-60kHz, microwave and ultrasonic synergistic treatment for 10-15 minutes, during which the temperature of the extraction system is controlled at 50-60℃. S4: Multi-stage filtration and purification The extracted mixture is first filtered through a 200-mesh filter cloth, and the initial filtrate is collected. Then, the initial filtrate is filtered through a ceramic membrane with a pore size of 0.2-0.4 μm and an operating pressure of 0.2-0.3 MPa, and the membrane filtrate is collected. S5: Concentrated Crystallization The membrane filtrate was placed in a rotary evaporator and concentrated to 1 / 5 to 1 / 4 of its original volume under a vacuum of 0.08-0.09 MPa and a temperature of 60-70℃ to obtain a concentrated solution. 3-5 times the volume of acetone was added to the concentrated solution, and after stirring evenly, it was placed in a refrigerated environment at 4-8℃ for 8-12 hours to crystallize. S6: Separation and Drying The crystallized mixture was centrifuged at 4000-5000 r / min for 10-15 min, and the precipitate was collected. The precipitate was placed in a vacuum drying oven and dried at 50-60℃ and 0.07-0.08 MPa for 3-4 h to obtain matrine product.

2. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, The specific parameters for the freezing-thawing operation in step S1 are as follows: first freezing temperature -20℃, freezing time 2.5h, thawing temperature 40℃, thawing time 1.2h; second freezing temperature -20℃, freezing time 2h, thawing temperature 40℃, thawing time 1h.

3. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, In step S2, the volume ratio of the composite impregnation solution is ethanol solution: sodium citrate solution = 9:1, the solid-liquid ratio is 1:20 (g / mL), the stirring and impregnation temperature is 28℃, the stirring speed is 180r / min, and the time is 35min; after mixing, the mixture is stirred and impregnated at 25-30℃ and 150-200r / min for 30-40min.

4. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, In step S3, the specific parameters for microwave-assisted ultrasound are as follows: microwave power 350W, frequency 2450MHz, microwave treatment alone for 6 minutes; then ultrasound power 180W, frequency 50kHz, and assisted treatment for 12 minutes are turned on simultaneously. During the assisted treatment, the system temperature is controlled at 55℃ by a constant temperature jacket.

5. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, In step S4, the ceramic membrane filter has a pore size of 0.3 μm and an operating pressure of 0.25 MPa.

6. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, In step S5, the rotary evaporation is carried out at a vacuum of 0.085 MPa and a temperature of 65°C, concentrating the liquid to 1 / 4 of its original volume; the amount of acetone added is 4 times the volume of the concentrated liquid, the refrigeration temperature is 6°C, and the liquid is allowed to stand for crystallization for 10 hours.

7. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, In step S6, the centrifugation speed is 4500 r / min and the time is 12 min; the vacuum drying temperature is 55℃, the vacuum degree is 0.075 MPa, and the drying time is 3.5 h.

8. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, In step S2, 0.1-0.2 g / L of disodium EDTA can also be added to the composite impregnation solution to improve the dissolution efficiency of matrine in Sophora flavescens powder.

9. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, In step S3, the microwave treatment time can be adjusted according to the moisture content of the Sophora flavescens powder: when the moisture content is ≤8%, the microwave treatment time is extended to 7-8 min; when the moisture content is >8%, the microwave treatment time is shortened to 5-6 min.

10. The method for efficient extraction of matrine based on microwave-assisted ultrasound as described in claim 1, characterized in that, In step S5, if the purity of the concentrate is low, the concentrate can be purified by adsorption with a macroporous resin before adding acetone. The macroporous resin is of type D101, the adsorption temperature is 25-30℃, the flow rate is 1-2 BV / h, and then eluted with a 70-80% ethanol solution. The eluent is collected and then concentrated by rotation.