A method for improving transfer rate of tanshinone ⅡA and application of the method

Abstract

The application provides a salvia miltiorrhiza extraction and concentration method for improving the transfer rate of tanshinone ⅡA and application, and relates to the technical field of traditional Chinese medicine preparation. The salvia miltiorrhiza extraction and concentration method for improving the transfer rate of tanshinone ⅡA comprises the following steps: selecting salvia miltiorrhiza medicinal materials, cleaning and crushing the salvia miltiorrhiza medicinal materials to obtain salvia miltiorrhiza powder; adding the salvia miltiorrhiza powder into a composite solvent according to a material-liquid ratio of 1:8-1:12, and performing ultrasonic-continuous reflux extraction; filtering the extraction liquid through filter paper or a filter screen, collecting and combining the filtrates obtained through multiple extractions; concentrating the filtrate; loading the concentrated filtrate onto a silica gel column, performing gradient elution using an eluent, and collecting the eluent containing tanshinone ⅡA; and transferring the eluent to a thin film evaporator, and performing thin film concentration until the formation of a extract-like product. The application improves the content and transfer rate of the product, thereby providing more abundant resources for the further application of tanshinone ⅡA.

Description

Technical Field

[0001] This invention relates to the field of traditional Chinese medicine preparation technology, specifically to a method for extracting and concentrating tanshinone IIA and its application. Background Technology

[0002] Danshen Injection, produced by Changshu Lei Yunshang Pharmaceutical Co., Ltd., has the effects of promoting blood circulation, removing blood stasis, clearing the meridians and nourishing the heart. It is widely used in clinical practice for chest tightness and angina pectoris caused by coronary heart disease and has significant therapeutic effects.

[0003] Danshen contains a variety of active ingredients, among which tanshinone IIA, as one of the main fat-soluble active ingredients of danshen, has significant cardiovascular pharmacological activities, such as improving myocardial ischemia and inhibiting platelet aggregation. Its content and transfer rate are crucial to the quality and efficacy of danshen-related preparations.

[0004] Traditional methods for extracting tanshinone have many drawbacks, such as low extraction rates, significant losses of tanshinone IIA during extraction and concentration, and low transfer rates. These issues result in the final product failing to achieve the desired levels of active ingredients, limiting the more efficient application of tanshinone in pharmaceuticals and health products. Therefore, developing an extraction and concentration method that can significantly improve the transfer rate of tanshinone IIA is urgently needed. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a method for extracting and concentrating tanshinone IIA and its application, thereby improving the transfer rate of tanshinone IIA and solving the problems mentioned in the background art.

[0006] To achieve the above objectives, the present invention provides the following technical solution: a method for extracting and concentrating tanshinone IIA to improve its transfer rate, comprising the following steps: Step 1: Pre-treatment of medicinal materials: The raw material of Salvia miltiorrhiza is selected, and after washing to remove mud and impurities, it is dried to constant weight at 40-60℃, and then pulverized to obtain Salvia miltiorrhiza powder. Step 2: Extraction: The danshen powder is added to a composite solvent at a material-to-liquid ratio of 1:8 to 1:12. The composite solvent is composed of 80% to 90% by volume of dichloroethanol and choline-based eutectic solvent at a volume ratio of 4 to 6:1. The mixture is then subjected to ultrasonic extraction 1 to 2 times at 50 to 100°C, followed by continuous reflux extraction. Step 3: Solid-liquid separation: After extraction, immediately filter the extract while it is still hot using filter paper or a filter screen, and collect and combine the filtrates obtained from multiple extractions; Step 4: Reduced pressure concentration: Place the filtrate in a vacuum concentration device, control the concentration temperature in the range of 45 to 55°C, maintain the pressure between -0.08 and -0.06 MPa, and continue the concentration operation until the volume of the filtrate is reduced to 1 / 4 to 1 / 3 of the original volume. Step 5: Column chromatography separation: The concentrated filtrate was loaded onto a silica gel column and eluted using a gradient elution method. The eluent containing tanshinone IIA was collected. Step Six: Thin-film Concentration The eluent was transferred to a thin-film evaporator, the evaporation temperature was set in the range of 60 to 70°C, the scraper speed was adjusted to 100 to 150 r / min, and the vacuum degree was controlled at -0.09 to -0.08 MPa. Thin-film concentration was carried out until a paste-like product was formed. Step 7: Drying The concentrated extract was further dried using vacuum drying or spray drying to obtain the tanshinone extract.

[0007] Preferably, in step one, the mesh size of the danshen powder is 20 to 60 mesh.

[0008] Preferably, in step two, the composite solvent is prepared by mixing 85% by volume dichloroethanol and a choline-based eutectic solvent at a volume ratio of 5:1.

[0009] Preferably, in step two, the ultrasonic power is set to 200-400W, the ultrasonic frequency is 30-50kHz, the extraction operation is repeated 3-5 times, and the extraction time for each extraction is 30-60 minutes.

[0010] Preferably, in step three, the mesh size of the filter paper or filter screen is 200 to 300 mesh.

[0011] Preferably, in step five, the silica gel particles in the silica gel column have a particle size of 100-200 mesh, and the ratio of column height to inner diameter is 8-12:1.

[0012] Preferably, in step five, the eluent is a petroleum ether-acetone mixed solution with a volume ratio of 6-9:1-4.

[0013] Preferably, in step five, the eluent is a dichloroethanol-water solution with a volume concentration of 30% to 70%.

[0014] This invention further discloses the application of the method for extracting and concentrating tanshinone IIA to improve its transfer rate in the preparation of tanshinone dripping pills.

[0015] This invention provides a method for extracting and concentrating tanshinone IIA and its application, which improves the transfer rate of tanshinone IIA. It has the following beneficial effects: 1. Through extensive experimental screening, this invention creatively uses dichloroethanol and choline-based eutectic solvents as extraction solvents, employs ultrasonic extraction and continuous reflux technology, combined with thin-film concentration process, which can significantly improve the extraction efficiency of tanshinone IIA, increasing its transfer rate by 20% to 30% compared to traditional extraction methods.

[0016] 2. During the concentration process, a vacuum concentration combined with a thin-film evaporator is used, which effectively reduces the loss of tanshinone IIA during the concentration process and ensures the content of active ingredients. Attached Figure Description

[0017] Figure 1 This is a schematic diagram of the process of the present invention. Detailed Implementation

[0018] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention. Example

[0019] like Figure 1 As shown, this embodiment of the invention provides a method for extracting and concentrating tanshinone IIA to improve its transfer rate, comprising the following steps: Step 1: Pre-treatment of medicinal materials: The raw material of Salvia miltiorrhiza is selected, and after washing to remove mud and impurities, it is dried at 40°C to constant weight. Then it is pulverized to obtain Salvia miltiorrhiza powder with a mesh size of 20 mesh. Step 2: Extraction: Add the danshen powder to the compound solvent at a material-to-liquid ratio of 1:8. The compound solvent (composed of 80% by volume of dichloroethanol and choline-based eutectic solvent at a volume ratio of 4:1) is used for ultrasonic-assisted extraction at 50°C. The ultrasonic power is set to 200W and the ultrasonic frequency is 30kHz. The extraction operation is repeated 3 times, with each extraction lasting 30 minutes. After ultrasonic extraction, add 10 times the amount of compound solvent and perform continuous reflux extraction twice, each time for 60 minutes.

[0020] Step 3: Solid-liquid separation: After extraction, combine the extracts and immediately filter them while they are still hot using filter paper or a 200-mesh filter screen. Collect and combine the filtrates obtained from multiple extractions. Step 4: Reduced pressure concentration: Place the filtrate in a vacuum concentration device, control the concentration temperature within the range of 45℃, maintain the pressure between -0.08MPa, and continue the concentration operation until the volume of the filtrate is reduced to 1 / 4 of the original volume. Step 5: Column chromatography separation: The concentrated filtrate was loaded onto a silica gel column with a silica gel particle size of 100 mesh and a column height to inner diameter ratio of 8:1. Gradient elution was performed using an eluent, specifically a petroleum ether-acetone mixture with a volume ratio of 6:1. The eluent containing tanshinone IIA was collected. Step Six: Thin-film Concentration The eluent was transferred to a thin-film evaporator, the evaporation temperature was set in the range of 60°C, the scraper speed was adjusted to 100 r / min, and the vacuum degree was controlled at -0.09 MPa. Thin-film concentration was carried out until a paste-like product was formed. Step 7: Drying The concentrated extract was further dried using vacuum drying or spray drying to obtain the tanshinone extract. Example

[0021] like Figure 1 As shown, this embodiment of the invention provides a method for extracting and concentrating tanshinone IIA to improve its transfer rate, comprising the following steps: Step 1: Pre-treatment of medicinal materials: The raw material of Salvia miltiorrhiza is selected, and after washing to remove mud and impurities, it is dried at 50°C to constant weight. Then it is pulverized to obtain Salvia miltiorrhiza powder with a mesh size of 40 mesh. Step 2: Extraction: Add the danshen powder to the compound solvent at a material-to-liquid ratio of 1:10. The compound solvent (composed of 85% by volume of dichloroethanol and choline-based eutectic solvent at a volume ratio of 5:1) is used for ultrasonic-assisted extraction at 60°C. The ultrasonic power is set to 300W and the ultrasonic frequency is 40kHz. The extraction operation is repeated 4 times, with each extraction lasting 45 minutes. After the ultrasonic extraction is completed, add 10 times the amount of compound solvent and perform continuous reflux extraction twice, each time for 60 minutes.

[0022] Step 3: Solid-liquid separation: After extraction, combine the extracts and immediately filter them while they are still hot using filter paper or a 250-mesh filter screen. Collect and combine the filtrates obtained from multiple extractions. Step 4: Reduced pressure concentration: Place the filtrate in a vacuum concentration device, control the concentration temperature within the range of 50℃, maintain the pressure between -0.07MPa, and continue the concentration operation until the volume of the filtrate is reduced to 1 / 4 of the original volume. Step 5: Column chromatography separation: The concentrated filtrate was loaded onto a silica gel column with a silica gel particle size of 150 mesh and a column height to inner diameter ratio of 10:1. Gradient elution was performed using an eluent, specifically a petroleum ether-acetone mixture with a volume ratio of 7:2. The eluent containing tanshinone IIA was collected. Step Six: Thin-film Concentration The eluent was transferred to a thin-film evaporator, the evaporation temperature was set in the range of 65°C, the scraper speed was adjusted to 120 r / min, and the vacuum degree was controlled at -0.085 MPa. Thin-film concentration was carried out until a paste-like product was formed. Step 7: Drying The concentrated extract was further dried using vacuum drying or spray drying to obtain the tanshinone extract. Example

[0023] like Figure 1 As shown, this embodiment of the invention provides a method for extracting and concentrating tanshinone IIA to improve its transfer rate, comprising the following steps: Step 1: Pre-treatment of medicinal materials: The raw material of Salvia miltiorrhiza is selected, and after washing to remove mud and impurities, it is dried at 60°C to constant weight. Then it is pulverized to obtain Salvia miltiorrhiza powder with a mesh size of 60 mesh. Step 2: Extraction: At a material-to-liquid ratio of 1:12, danshen powder was added to a compound solvent, which was a mixture of 90% by volume dichloroethanol and a choline-based eutectic solvent at a volume ratio of 6:1. Ultrasonic-assisted extraction was performed at 70°C, with the ultrasonic power set at 400W and the ultrasonic frequency at 50kHz. The extraction was repeated 5 times, with each extraction lasting 60 minutes. After ultrasonic extraction, 12 times the amount of compound solvent was added and continuous reflux extraction was performed 3 times, each time for 45 minutes.

[0024] Step 3: Solid-liquid separation: After extraction, immediately filter the extract while it is still hot using filter paper or a 300-mesh filter screen. Collect and combine the filtrates obtained from multiple extractions. Step 4: Reduced pressure concentration: Place the filtrate in a vacuum concentration device, control the concentration temperature within the range of 55℃, maintain the pressure between -0.06MPa, and continue the concentration operation until the volume of the filtrate is reduced to 1 / 3 of the original volume. Step 5: Column chromatography separation: The concentrated filtrate was loaded onto a silica gel column with a silica gel particle size of 200 mesh and a column height to inner diameter ratio of 12:1. Gradient elution was performed using an eluent, specifically a petroleum ether-acetone mixture with a volume ratio of 9:4. The eluent containing tanshinone IIA was collected. Step Six: Thin-film Concentration The eluent was transferred to a thin-film evaporator, the evaporation temperature was set in the range of 70°C, the scraper speed was adjusted to 150 r / min, and the vacuum degree was controlled at -0.08 MPa. Thin-film concentration was carried out until a paste-like product was formed. Step 7: Drying The concentrated extract was further dried using vacuum drying or spray drying to obtain the tanshinone extract. Example

[0025] The difference between this embodiment and Embodiment 1 is that, in step five, the eluent is an ethanol-water solution with a volume concentration of 30%. Example

[0026] The difference between this embodiment and Embodiment 1 is that, in step five, the eluent is an ethanol-water solution with a volume concentration of 50%. Example

[0027] The difference between this embodiment and Embodiment 1 is that, in step five, the eluent is an ethanol-water solution with a volume concentration of 70%.

[0028] Comparative Example 1: A method for extracting and concentrating tanshinone IIA to improve its transfer rate includes the following steps: Step 1: Pre-treatment of medicinal materials: The raw material of Salvia miltiorrhiza is selected, and after washing to remove mud and impurities, it is dried at 40°C to constant weight. Then it is pulverized to obtain Salvia miltiorrhiza powder with a mesh size of 20 mesh. Step 2: Extraction: Add 80% ethanol to the salvia powder at a material-to-liquid ratio of 1:8, and perform ultrasonic-assisted extraction at 50°C. The ultrasonic power is set to 200W and the ultrasonic frequency is 30kHz. The extraction operation is repeated 3 times, with each extraction lasting 30 minutes. Step 3: Solid-liquid separation: After extraction, immediately filter the extract while it is still hot using filter paper or a 200-mesh filter screen. Collect and combine the filtrates obtained from multiple extractions. Step 4: Column Chromatography Separation: The above filtrate was loaded onto a silica gel column with a silica gel particle size of 100 mesh and a column height to inner diameter ratio of 8:1. Gradient elution was performed using an eluent, specifically a petroleum ether-acetone mixture with a volume ratio of 6:1. The eluent containing tanshinone IIA was collected. Step 5: Drying The above eluent was further dried using vacuum drying or spray drying to obtain the tanshinone extract.

[0029] Experiment Example 7: The content of tanshinone IIA in Examples 1 to 6 and Comparative Example 1 was detected.

[0030] In summary, in the embodiments of the present invention, the content and transfer rate of tanshinone IIA were significantly higher than those in the comparative example, indicating that the method of the present invention can effectively improve the extraction efficiency and transfer rate of tanshinone IIA. Specifically, in Examples 1 to 6, the content of tanshinone IIA was all above 3.17 mg / g, and the transfer rate was all above 77.9%, while in the comparative example, the content of tanshinone IIA was only 2.01 mg / g, and the transfer rate was only 57.8%. This shows that the extraction and concentration method of the present invention, while maintaining the stability of tanshinone IIA, significantly improves its content and transfer rate in the final product, thus providing a richer resource for the further application of tanshinone IIA.

[0031] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A method for extracting and concentrating tanshinone IIA to improve its transfer rate, characterized in that: Includes the following steps: Step 1: Pre-treatment of medicinal materials: The raw material of Salvia miltiorrhiza is selected, and after washing to remove mud and impurities, it is dried to constant weight at 40-60℃, and then pulverized to obtain Salvia miltiorrhiza powder. Step 2: Extraction: The danshen powder was added to a composite solvent at a material-to-liquid ratio of 1:8 to 1:

12. The composite solvent was composed of 80% to 90% by volume of dichloroethanol and choline-based eutectic solvent at a volume ratio of 4 to 6:

1. The mixture was subjected to ultrasonic extraction at 50 to 100°C, followed by continuous reflux extraction. Step 3: Solid-liquid separation: After extraction, immediately filter the extract while it is still hot using filter paper or a filter screen, and collect and combine the filtrates obtained from multiple extractions; Step 4: Reduced pressure concentration: Place the filtrate in a vacuum concentration device, control the concentration temperature in the range of 45 to 55°C, maintain the pressure between -0.08 and -0.06 MPa, and continue the concentration operation until the volume of the filtrate is reduced to 1 / 4 to 1 / 3 of the original volume. Step 5: Column chromatography separation: The concentrated filtrate was loaded onto a silica gel column and eluted using a gradient elution method. The eluent containing tanshinone IIA was collected. Step Six: Thin-film Concentration The eluent was transferred to a thin-film evaporator, the evaporation temperature was set in the range of 60 to 70°C, the scraper speed was adjusted to 100 to 150 r / min, and the vacuum degree was controlled at -0.09 to -0.08 MPa. Thin-film concentration was carried out until a paste-like product was formed. Step 7: Drying The concentrated extract was further dried using vacuum drying or spray drying to obtain the tanshinone extract.

2. The method for improving the transfer rate of tanshinone IIA according to claim 1, characterized in that: In step one, the mesh size of the danshen powder is 20-60 mesh.

3. The method for improving the transfer rate of tanshinone II A according to claim 1, characterized in that: In step two, the composite solvent is prepared by mixing dichloroethanol (85% by volume) and choline-based eutectic solvent at a volume ratio of 5:

1.

4. The method for extracting and concentrating tanshinone IIA to improve the transfer rate of tanshinone as described in claim 3, characterized in that: In step two, the ultrasonic power is set to 200-400W, the ultrasonic frequency is 30-50kHz, the extraction operation is repeated 3-5 times, and the extraction time for each extraction is 30-60 minutes.

5. The method for extracting and concentrating tanshinone IIA to improve the transfer rate of tanshinone as described in claim 1, characterized in that: In step three, the filter paper or filter screen has a mesh size of 200 to 300.

6. The method for extracting and concentrating tanshinone IIA to improve the transfer rate of tanshinone as described in claim 1, characterized in that: In step five, the silica gel particles in the silica gel column have a particle size of 100-200 mesh, and the ratio of column height to inner diameter is 8-12:

1.

7. The method for extracting and concentrating tanshinone IIA to improve the transfer rate of tanshinone as described in claim 6, characterized in that: In step five, the eluent is a petroleum ether-acetone mixed solution with a volume ratio of 6-9:1-4.

8. The method for extracting and concentrating tanshinone IIA to improve the transfer rate of tanshinone as described in claim 6, characterized in that: In step five, the eluent is a dichloroethanol-water solution with a volume concentration of 30% to 70%.

9. The application of the method for extracting and concentrating tanshinone IIA according to any one of claims 1-8 in the preparation of tanshinone injection.

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