Method for efficiently extracting total alkaloids of sophora alopecuroides
By adjusting the pH value of bitter bean extract and enriching with pretreated cationic resin fillers, the problem of low extraction rate of total alkaloids in bitter beans is solved, and the efficiency of extracting total alkaloids in bitter beans is achieved, and the yield and purity are significantly improved.
Patent Information
- Application Number
- CN202411680076.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Applications(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-22
- Publication Date
- 2025-02-28
AI Technical Summary
In the prior art, the extraction rate of total alkaloids in bitter beans is relatively low, and it is difficult to meet the demand for efficient extraction.
A method for efficient extraction of total alkaloids of bitter beans is adopted, including obtaining a concentrate of total extract of bitter beans, adjusting its pH value to 9 or more, enriching with pretreated 732 and 001 cationic resin fillers, generating alkaloid salts through acid-base reactions, and improving extraction efficiency through elution and alkalinization processes.
The efficient extraction of total alkaloids of bitter beans was achieved, with an average yield of 11.8%, and a purity of more than 98%, which significantly improved the extraction rate and purity in the prior art.
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Figure CN119524038A_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of alkaloid extraction, and particularly relates to a method for efficiently extracting total alkaloids from sophora alopecuroides. Background Art
[0002] Sophora alopecuraides L. is a plant of the genus Sophora in the Leguminosae family. It is also known as bitter liquorice, bitter bean root, western bean root, and bitter ginseng grass. my country is the main country for the cultivation and use of bitter bean medicinal materials, and its production accounts for about 62% of the world. Sophora alopecura is one of the six major traditional Chinese medicinal materials protected by the Ningxia Hui Autonomous Region. It is mainly distributed in Yanchi County, Wuzhong City, and has rich resources.
[0003] Sophora alopecuroides contains many types of compounds, among which alkaloids are the main components that exert various pharmacological effects. For example, matrine has anti-nephritis, hepatitis, skin inflammation, and anti-colorectal cancer activities; sophora alopecuroides has the activities of improving human bronchial epithelial cell damage and regulating prostate cancer cell autophagy. In addition, sophora alopecuroides alkaloids are also used clinically to treat diseases, such as total sophora alopecuroides alkaloids can treat radiation skin damage. Therefore, sophora alopecuroides alkaloids have a wide range of uses.
[0004] The Chinese invention patent with patent number CN101912438A discloses a process for extracting total alkaloids from Sophora alopecuroides. The process includes crushing, warm extraction, clarification, alkalization extraction, acidification displacement extraction, microwave vacuum drying, etc. to obtain dry total alkaloid powder from Sophora alopecuroides. The total alkaloid yield is 5.7%. It can be seen that the extraction rate of total alkaloids is low. Summary of the invention
[0005] In view of this, the present invention provides an application of total alkaloids from Sophora alopecuroides and a method for efficiently extracting total alkaloids from Sophora alopecuroides, so as to solve the technical problem of low extraction rate of total alkaloids from Sophora alopecuroides in the prior art.
[0006] To achieve the above objectives, this application adopts the following scheme:
[0007] A method for efficiently extracting total alkaloids from Sophora alopecuroides comprises the following steps:
[0008] S10. Obtaining a concentrated solution of the total extract of Sophora alopecuroides;
[0009] S20. extracting the concentrated solution to obtain a sample solution;
[0010] S30. adjusting the pH of the sample solution to be greater than or equal to 9;
[0011] S40. Prepare a resin filler, and pre-treat the resin filler, and use the pre-treated resin filler to enrich the total alkaloids in the sample solution: contact the sample solution with a pH of greater than or equal to 9 with the resin filler for a first reaction time, so that the alkaloid compounds in the sample solution react to form alkaloid salts, and the alkaloid salts are adsorbed on the surface of the resin filler, and the sample solution is eluted with water to wash away the unreacted non-alkaloids in the sample solution, and after elution, the alkaloid salts are alkalized with 20% to 30% ammonia water to alkalize the alkaloid salts into alkaloids, and the alkaloids are eluted with 8% to 12% ammonia water to obtain a total alkaloid solution, wherein the resin filler includes 732 type cationic resin and 001 type cationic resin;
[0012] S50. taking the total alkaloid solution, recovering the solvent, vacuum drying and then crushing to obtain the sophora alopecuroides total alkaloid powder.
[0013] Preferably, the solid-liquid ratio of the resin filler to the sample liquid is (40 g to 60 g):5 mL.
[0014] Preferably, the first duration is from 11 hours to 12 hours.
[0015] Preferably, the mass ratio of the 732 type cationic resin to the 001 type cationic resin is (7:3) to (9:1).
[0016] Preferably, the step S10 includes the following steps:
[0017] S11. Grind the seeds, roots, stems and leaves of bitter bean into coarse powder and pass through a 30-mesh sieve;
[0018] S12. Pre-soak the coarse powder in a hydrochloric acid aqueous solution with a pH of 2 to 3 for 12 h ± 2 h, then ultrasonically extract at least 4 times, each extraction for 2 h ± 1 h, obtain a filtrate each time, combine the filtrate obtained from each extraction, and the solid-liquid ratio of the coarse powder to the hydrochloric acid aqueous solution is 1: (7 to 9);
[0019] S13. Concentrate the combined filtrates to obtain a concentrated solution.
[0020] Preferably, the step S20 comprises: extracting the concentrated solution with an ethyl acetate solution: mixing the concentrated solution with the ethyl acetate solution, and taking out a lower water layer after stratification, wherein the lower water layer is the sample solution.
[0021] Preferably, the mass ratio of the concentrated solution to the ethyl acetate solution is 1:1.
[0022] Preferably, the pretreatment of the resin filler in step S40 includes the following steps:
[0023] S41. Rinse the resin filler with pure water until it is colorless;
[0024] S42. Soak the resin filler in the step S41 for 3h to 4h using a 1mol / L to 2mol / L aqueous hydrochloric acid solution;
[0025] S43. Rinse the resin filler in step S42 to neutrality using pure water;
[0026] S44. Soak the resin filler in the step S43 for 1 h to 2 h using 1 mol / L to 3 mol / L NaOH solution;
[0027] S45. Rinse the resin filler in step S44 to neutrality using pure water;
[0028] S46. Soak the resin filler in the step S45 for 1 h to 2 h using a 1 mol / L to 2 mol / L hydrochloric acid aqueous solution;
[0029] S47. Wash the resin filler in step S46 with pure water until the pH is 5 to 6;
[0030] S48. Load the resin filler in step S47 into a column.
[0031] The technical solution adopted in this application can achieve the following beneficial effects:
[0032] The present invention provides a method for efficiently extracting total alkaloids from Sophora alopecuroides. First, a concentrated solution of total extracts from Sophora alopecuroides is obtained, and its volume is reduced to facilitate extraction; the concentrated solution is extracted to obtain a sample solution, and the pH of the sample solution is adjusted to be greater than or equal to 9, so that the sample solution is alkaline, so that alkaloid compounds are more easily replaced from the original solution; a resin filler is prepared, and the resin filler is pretreated to remove inorganic impurities such as iron compounds, calcium and magnesium ions in the resin, and the total alkaloids in the sample solution are enriched using the pretreated resin filler: the sample solution with a pH greater than or equal to 9 is contacted with the resin filler for a first reaction time, the 732-type cationic resin in the pretreated resin filler can react with most of the alkaloid compounds in the sample solution, and the 001-type cationic resin in the resin filler can react with a small part of the alkaloid compounds in the sample solution, and the reaction generates Alkaloid salts, the resin filler can adsorb and retain the alkaloid salts in the sample solution, so that the alkaloid salts are attached to the resin filler, the sample solution is eluted with water to wash away the unreacted non-alkaloids in the sample solution, the alkaloid salts are alkalized with 20% to 30% ammonia water after elution, the alkaloid salts are alkalized into alkaloids, and the alkaloids are eluted with 8% to 12% ammonia water to obtain a total alkaloid solution, and the resin filler can also effectively remove impurities in the sample solution during the enrichment process to improve the purity of the total alkaloids. The average yield of total alkaloids extracted from Sophora alopecuroides by the method provided by the application is 11.8%, and the purity is above 98%. Compared with the method for extracting total alkaloids from Sophora alopecuroides disclosed in the prior art, the method provided by the application can efficiently extract total alkaloids from Sophora alopecuroides with higher purity, which is 6.1% higher than the yield of total alkaloids extracted from Sophora alopecuroides in the prior art, which is increased by 2 times, and has significant beneficial effects.
[0033] The resin filler in the method provided in the present application is a recyclable material, which can be reused in industrial production and can also reduce production costs. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] Figure 1 It is a process flow chart of the present invention. DETAILED DESCRIPTION
[0035] In order to facilitate the understanding of the present application, the present application will be described more comprehensively below in conjunction with the accompanying drawings. And the preferred implementation of the present application is given. However, the present application can be implemented in many different forms and is not limited to the implementation described herein. On the contrary, the purpose of providing these implementations is to make the disclosure of the present application more thoroughly and comprehensively understood.
[0036] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those generally understood by those skilled in the art to which this application belongs. The terms used herein in the specification of this application are only for the purpose of describing specific embodiments and are not intended to limit this application. The term "and / or" used herein includes any and all combinations of one or more related listed items.
[0037] A method for efficiently extracting total alkaloids from Sophora alopecuroides comprises the following steps:
[0038] S10. Obtaining a concentrated solution of the total extract of Sophora alopecuroides;
[0039] S20. extracting the concentrated solution to obtain a sample solution;
[0040] S30. adjusting the pH of the sample solution to be greater than or equal to 9;
[0041] S40. Prepare a resin filler, and pre-treat the resin filler, and use the pre-treated resin filler to enrich the total alkaloids in the sample solution: contact the sample solution with a pH of greater than or equal to 9 with the resin filler for a first reaction time, so that the alkaloid compounds in the sample solution react to form alkaloid salts, and the alkaloid salts are adsorbed on the surface of the resin filler, and the sample solution is eluted with water to wash away the unreacted non-alkaloids in the sample solution, and after elution, the alkaloid salts are alkalized with 20% to 30% ammonia water to alkalize the alkaloid salts into alkaloids, and the alkaloids are eluted with 8% to 12% ammonia water to obtain a total alkaloid solution, wherein the resin filler includes 732 type cationic resin and 001 type cationic resin;
[0042] S50. taking the total alkaloid solution, recovering the solvent, vacuum drying and then crushing to obtain the sophora alopecuroides total alkaloid powder.
[0043] In this embodiment, the seeds, roots, stems and leaves of Sophora alopecuroides, or a combination thereof, can be used to prepare a concentrated solution of Sophora alopecuroides. Concentration can reduce the volume and weight of the extract, which is convenient for subsequent steps. The concentrated solution is extracted. Impurities in the concentrated solution can be effectively removed through extraction to obtain a sample solution. The sample solution is alkalized and the pH of the sample solution is adjusted to be greater than or equal to 9. In this embodiment, an 8% sodium hydroxide solution is used to adjust the pH of the sample solution so that the sample solution is alkaline. The pretreated resin filler is acidic. When the pretreated resin filler contacts and reacts with the sample solution, the alkaloid compounds are more easily released from the original solution through the acid-base reaction.
[0044] When the method provided by the present application is used to extract the total alkaloids of Sophora alopecuroides, the pretreated resin filler is used to enrich the total alkaloids in Sophora alopecuroides, the pretreated resin filler has removed inorganic impurities such as iron compounds, calcium and magnesium ions in the resin, and the resin filler is converted into a hydrogen filler, the 732-type cationic resin in the pretreated resin filler can react with most of the alkaloid compounds in the sample solution, the 001-type cationic resin in the resin filler can react with a small part of the alkaloid compounds in the sample solution to react to generate alkaloid salts, and the resin filler can adsorb and retain the alkaloid compounds in the sample solution, thereby extracting The concentration of high alkaloid compounds is high. The resin filler can also effectively remove impurities in the sample solution during the enrichment process, thereby improving the purity of the alkaloid compounds. The average yield of total alkaloids extracted from Sophora alopecuroides by the method provided in the present application is 11.8%, and the purity is above 98%. Compared with the method for extracting total alkaloids from Sophora alopecuroides disclosed in the prior art, the method provided in the present application can efficiently extract total alkaloids from Sophora alopecuroides with higher purity, which is 6.1% higher than the yield of total alkaloids extracted from Sophora alopecuroides in the prior art, which is increased by 2 times and has significant beneficial effects. In addition, the resin filler is a recyclable material and can be reused in industrial production, thereby reducing production costs.
[0045] Wherein, the solid-liquid ratio of the resin filler to the sample liquid is (40g to 60g): 5mL. If the resin filler is excessive, it will cause blockage or excessive dilution of the sample liquid, affecting the enrichment quality. If the resin filler is insufficient, the sample liquid and the resin filler will not react sufficiently. Therefore, when the solid-liquid ratio of the resin filler to the sample liquid is (40g to 60g): 5ml, it can ensure that the resin filler is fully in contact with the alkaloid compounds in the sample liquid, thereby improving the enrichment efficiency, and can also reduce the waste of the resin filler and the amount of the sample liquid, thereby saving costs and resources.
[0046] Among them, the first time length is 11 hours to 12 hours. If the first time length is less than 11 hours, the sample liquid and the resin filler will not react fully. If the first time length is greater than 12 hours, the sample liquid and the resin filler will basically no longer react. That is to say, when the first time length is 11 hours to 12 hours, the sample liquid and the resin filler can fully react.
[0047] Preferably, the mass ratio of the 732 type cationic resin to the 001 type cationic resin is (7:3) to (9:1).
[0048] In some specific embodiments, the step S10 includes the following steps:
[0049] S11. Grind the seeds, roots, stems and leaves of bitter bean into coarse powder and pass through a 30-mesh sieve;
[0050] S12. Pre-soak the coarse powder in a hydrochloric acid aqueous solution with a pH of 2 to 3 for 12 h ± 2 h, then ultrasonically extract at least 4 times, each extraction for 2 h ± 1 h, obtain a filtrate each time, combine the filtrate obtained from each extraction, and the solid-liquid ratio of the coarse powder to the hydrochloric acid aqueous solution is 1: (7 to 9);
[0051] S13. Concentrate the combined filtrates to obtain a concentrated solution.
[0052] The seeds, roots, stems and leaves of bitter bean are all crushed into coarse powder and passed through a 30-mesh sieve. The powder is soaked in a hydrochloric acid aqueous solution to destroy the cell structure in the powder and fully dissolve the target substance (alkaloid) in the solution. Soaking for 12h±2h and multiple ultrasonic extractions can ensure that the alkaloid compounds are completely released from the powder and dissolved in the solution, thereby improving the extraction efficiency.
[0053] Furthermore, the step S20 includes: extracting the concentrated solution with an ethyl acetate solution: mixing the concentrated solution with the ethyl acetate solution, taking out the lower water layer after stratification, wherein the lower water layer is the sample solution, and using the ethyl acetate solution as the extraction solvent, thereby reducing the solvent recovery time and improving the extraction efficiency.
[0054] Wherein, the mass ratio of the concentrated solution to the ethyl acetate solution is 1:1.
[0055] In some preferred embodiments, the pretreatment of the resin filler in step S40 includes the following steps:
[0056] S41. Use pure water to rinse the resin filler until it becomes colorless, and wash away impurities attached to the surface of the filler, so that the extracted alkaloid has a higher purity.
[0057] S42. Soak the resin filler in the S41 step for 3 to 4 hours using a 1 mol / L to 2 mol / L hydrochloric acid aqueous solution, so that the resin filler is soaked in an acidic environment, and inorganic impurities, especially iron compounds, in the resin filler can be removed. Thereby improving the purity and stability of the resin filler, ensuring that it can exert its best performance during the contact reaction with the sample solution, and avoiding the interference of inorganic impurities with subsequent processing steps, affecting the quality and yield of total alkaloids.
[0058] S43. Use pure water to rinse the resin filler in step S42 until it becomes neutral, and wash away the residual hydrochloric acid solution in the previous step.
[0059] S44. Use 1mol / L to 3mol / LNaOH solution to soak the resin filler in the S43 step for 1h to 2h; soaking the resin filler in an alkaline environment can remove calcium and magnesium ions in the resin filler, and prevent calcium and magnesium ions from being transferred into the sample solution when the resin filler contacts and reacts with the sample solution, thereby affecting the quality of the extracted total alkaloids. Removing calcium and magnesium ions in the resin filler can also maintain the exchange capacity and performance of the resin filler and extend its service life.
[0060] S45. Use pure water to rinse the resin filler in step S44 to neutrality and wash away the residual alkali solution.
[0061] S46. Use 1 mol / L to 2 mol / L hydrochloric acid aqueous solution to soak the resin filler in the S45 step for 1 hour to 2 hours; convert the calcium type or other type of resin in the resin filler into a hydrogen type resin to better carry out a specific chemical reaction or ion exchange process. The surface charge of the hydrogen type resin is neutral, and it can better adsorb and remove cations in the solution, thereby improving the separation effect and the control of reaction conditions.
[0062] S47. Use pure water to wash the resin filler in step S46 to a pH of 5 to 6, so that the filler can react better with the sample solution.
[0063] S48. Load the resin filler in step S47 into a column.
[0064] The resin filler obtained by the treatment of step S41 to step S48 can adsorb and retain the alkaloid compounds in the sample liquid when it contacts and reacts with the sample liquid, thereby increasing the concentration of the alkaloid compounds. During the enrichment process, the resin filler can also effectively remove impurities in the sample liquid and improve the purity of the alkaloid compounds.
[0065] The method for efficiently extracting total alkaloids from Sophora alopecuroides provided by the present invention can quickly and effectively extract total alkaloids with high purity, can be widely used in drugs for preventing nephritis, hepatitis, skin inflammation and colorectal cancer, and plays an important role in the medical field.
[0066] The following specific experimental examples are used to further illustrate the technical solutions and technical effects of the present invention. It should be noted that the following experimental examples are only for further explaining the present invention and do not limit the technical solutions of the present invention.
[0067] Experimental Example 1
[0068] Test methods
[0069] In this Example 1, three groups of parallel experiments were used to extract total alkaloids from Sophora alopecuroides, and the yield of total alkaloids extracted in each experimental example was detected, and the average value of total alkaloids extracted from Sophora alopecuroides in the three groups of parallel experiments was calculated.
[0070] Experimental procedures
[0071] Prepare the sample solution: grind the seeds, roots, stems and leaves of Sophora alopecuroides into coarse powder and pass it through a 30-mesh sieve, pre-soak the coarse powder in a hydrochloric acid aqueous solution with a pH of 3 for 12 hours, then perform ultrasonic extraction 4 times, each time for 2 hours, combine the filtrates, filter under reduced pressure to obtain a filtrate, and concentrate the filtrate to obtain a concentrated solution; mix the concentrated solution with an ethyl acetate solution in a mass ratio of 1:1, let it stand, and take out the lower water layer after stratification, the lower water layer is the sample solution, and the pH of the sample solution is adjusted to be greater than or equal to 9.
[0072] Preparation of resin filler: Take 732 type cationic resin and 001 type cationic resin and mix them evenly in a mass ratio of 8:2 to obtain resin filler, and pretreat the resin filler: rinse the resin filler with pure water until it is colorless; soak the resin filler in 1mol / L hydrochloric acid aqueous solution for 4 hours, and wash the resin filler with pure water until it is neutral after soaking; then, soak the resin filler in 2mol / LNaOH solution for 1 hour, and wash it with pure water until it is neutral after soaking; soak the resin filler in 1mol / L hydrochloric acid aqueous solution for 2 hours, and wash it with pure water until the pH is 6 after soaking; finally, load the resin filler into the column.
[0073] The resin filler is used to enrich the total alkaloids in the sample solution: the sample solution is wet loaded, and the solid-liquid ratio of the resin filler to the sample solution is 50g:5mL; and the resin filler is contacted with the sample solution for reaction for 12h to generate alkaloid salts, and after the reaction, the sample solution is eluted with pure water for 3 to 4 column volumes; then, the alkaloids are alkalized with 25% ammonia water and immersed for 4h, and after the immersion, the alkaloids are eluted with 10% ammonia water, and the total alkaloid solution is obtained after elution, the solvent is recovered, and the powder is crushed after vacuum drying to obtain the total alkaloid powder of Sophora alopecuroides.
[0074] The yield and purity of the total alkaloids extracted from the three parallel experimental examples in the above Experimental Example 1 were tested by thin layer chromatography and ultraviolet spectrophotometry, and the test results are shown in Table 1.
[0075] Comparative Example 1
[0076] The difference between this comparative example 1 and the above experimental example 1 is that the 732 type cationic resin is used as a resin filler to enrich the sample solution, and the other steps and methods are the same as the steps and methods in the above experimental example 1. The yield and purity of the total alkaloids extracted in this comparative example 1 are detected by thin layer chromatography and ultraviolet spectrophotometry, respectively, and the test results are shown in Table 1.
[0077] Comparative Example 2
[0078] The difference between this comparative example 2 and the above experimental example 1 is that the 001 type cationic resin is used as a resin filler to enrich the sample solution, and the other steps and methods are the same as the steps and methods in the above experimental example 1. The yield and purity of the total alkaloids extracted in this comparative example 2 are detected by thin layer chromatography and ultraviolet spectrophotometry, respectively, and the test results are shown in Table 1.
[0079] Comparative Example 3
[0080] The difference between Experimental Example 3 and Experimental Example 1 is that: 732 type cationic resin and 001 type cationic resin are mixed uniformly in a mass ratio of 9:1 to obtain a resin filler, and the resin filler is directly loaded into a column to enrich the total alkaloids in the sample solution without pretreatment. The other steps and methods are the same as those in Experimental Example 1. The yield and purity of the total alkaloids extracted in Experimental Example 3 are detected by thin layer chromatography and ultraviolet spectrophotometry, respectively. The test results are shown in Table 1:
[0081] Table 1 Total alkaloid yield in Experimental Example 1 and Comparative Examples 1 to 3
[0082]
[0083] The data in Experimental Example 1 in Table 1 show that the average yield of total alkaloids extracted from Sophora alopecuroides by the method provided by the present application is 11.8%, and the purity is above 98%. Compared with the method for extracting total alkaloids from Sophora alopecuroides disclosed in the prior art, the method provided by the present application can efficiently extract total alkaloids from Sophora alopecuroides with higher purity, and the yield of total alkaloids extracted from Sophora alopecuroides by the method provided by the present application is 6.1% higher than that of the prior art, which is 2 times higher, and has significant beneficial effects;
[0084] It can be seen from the data in Comparative Examples 1 and 2 in Table 1 above that if the resin filler does not include the 001 type cationic resin, the yield of total alkaloids extracted from Sophora alopecuroides is not significantly improved compared to the yield of total alkaloids extracted from Sophora alopecuroides by the method in the prior art; if the resin filler does not include the 732 type cationic resin, the yield of total alkaloids extracted from Sophora alopecuroides is lower than the yield of total alkaloids extracted from Sophora alopecuroides by the method in the prior art;
[0085] The data in Comparative Example 3 in Table 1 above fully reflect that if the resin filler prepared by mixing Type 732 cationic resin and Type 001 cationic resin is not pretreated and is used to enrich the total alkaloids in Sophora alopecuroides, the yield and purity of the total alkaloids are only half of the yield and purity of the total alkaloids in Test Example 1.
[0086] In summary, the 732-type cationic resin and the 001-type cationic resin are mixed to prepare a resin filler, and the resin filler is pretreated. When the pretreated resin filler is used to enrich the total alkaloids in Sophora alopecuroides, the effect is better and has significant beneficial effects.
[0087] Experimental Example 2
[0088] The difference between Experimental Example 2 and Experimental Example 1 is that the mass ratio of the 732-type cationic resin to the 001-type cationic resin is changed to prepare the resin filler. The mass ratios of the 732-type cationic resin to the 001-type cationic resin are 4:6, 5:5, 6:4, 7:3, and 9:1, respectively. The other steps and methods are the same as those in Experimental Example 1. The yield and purity of the total alkaloids extracted in Experimental Example 2 are detected by thin layer chromatography and ultraviolet spectrophotometry, respectively. The test results are shown in Table 2.
[0089] Table 2 Total alkaloid yield in Experimental Example 2
[0090]
[0091] It can be seen from the data in Table 2 that when the content of the 732-type cationic resin in the resin filler is less, the yield of total alkaloids in Sophora alopecuroides enriched by using the resin filler is low, and the effect is better when the mass ratio of the 732-type cationic resin to the 001-type cationic resin in the resin filler is 8:2, and the effect is second only when the mass ratio of the 732-type cationic resin to the 001-type cationic resin in the resin filler is 9:1 and 7:3.
[0092] The above description is only a specific implementation mode of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can easily think of various equivalent modifications or substitutions within the technical scope disclosed by the present invention, and these modifications or substitutions should be included in the protection scope of the present invention.
Claims
1. A method for efficiently extracting total alkaloids from Sophora alopecuroides, characterized in that: The following steps are involved: S10. Obtaining a concentrated solution of the total extract of Sophora alopecuroides; S20. extracting the concentrated solution to obtain a sample solution; S30. adjusting the pH of the sample solution to be greater than or equal to 9; S40. Prepare a resin filler, and pre-treat the resin filler, and use the pre-treated resin filler to enrich the total alkaloids in the sample solution: contact the sample solution with a pH of greater than or equal to 9 with the resin filler for a first reaction time, so that the alkaloid compounds in the sample solution react to form alkaloid salts, and the alkaloid salts are adsorbed on the surface of the resin filler, and the sample solution is eluted with water to wash away the unreacted non-alkaloids in the sample solution, and after elution, the alkaloid salts are alkalized with 20% to 30% ammonia water to alkalize the alkaloid salts into alkaloids, and the alkaloids are eluted with 8% to 12% ammonia water to obtain a total alkaloid solution, wherein the resin filler includes 732 type cationic resin and 001 type cationic resin; S50. taking the total alkaloid solution, recovering the solvent, vacuum drying and then crushing to obtain the sophora alopecuroides total alkaloid powder.
2. The method for efficiently extracting total alkaloids from Sophora alopecuroides according to claim 1, characterized in that: The solid-to-liquid ratio of the resin filler to the sample liquid is (40 g to 60 g): 5 mL.
3. The method for efficiently extracting total alkaloids from Sophora alopecuroides according to claim 1, characterized in that: The first duration is from 11h to 12h.
4. The method for efficiently extracting total alkaloids from Sophora alopecuroides according to claim 1, characterized in that: The mass ratio of the 732 type cationic resin to the 001 type cationic resin is (7:3) to (9:1).
5. The method for efficiently extracting total alkaloids from Sophora alopecuroides according to claim 1, characterized in that: The step S10 comprises the following steps: S11. Grind the seeds, roots, stems and leaves of bitter bean into coarse powder and pass through a 30-mesh sieve; S12. Pre-soak the coarse powder in a hydrochloric acid aqueous solution with a pH of 2 to 3 for 12 h±2 h, then ultrasonically extract at least 4 times, each extraction for 2 h±1 h, obtain a filtrate each time, combine the filtrate obtained from each extraction, and the solid-liquid ratio of the coarse powder to the hydrochloric acid aqueous solution is 1: (7 to 9); S13. Concentrate the combined filtrates to obtain a concentrated solution.
6. The method for efficiently extracting total alkaloids from Sophora alopecuroides according to claim 1, characterized in that: The step S20 includes: extracting the concentrated solution with an ethyl acetate solution: mixing the concentrated solution with the ethyl acetate solution, and taking out a lower water layer after stratification, wherein the lower water layer is the sample solution.
7. The method for efficiently extracting total alkaloids from Sophora alopecuroides according to claim 6, characterized in that: The mass ratio of the concentrated solution to the ethyl acetate solution is 1:
1.
8. The method for efficiently extracting total alkaloids from Sophora alopecuroides according to claim 1, characterized in that: The pretreatment of the resin filler in step S40 includes the following steps: S41. Rinse the resin filler with pure water until it is colorless; S42. Soak the resin filler in the step S41 for 3h to 4h using a 1mol / L to 2mol / L aqueous hydrochloric acid solution; S43. Rinse the resin filler in step S42 to neutrality using pure water; S44. Soak the resin filler in the step S43 for 1 h to 2 h using 1 mol / L to 3 mol / L NaOH solution; S45. Rinse the resin filler in step S44 to neutrality using pure water; S46. Soak the resin filler in the step S45 for 1 h to 2 h using a 1 mol / L to 2 mol / L hydrochloric acid aqueous solution; S47. Wash the resin filler in step S46 with pure water until the pH is 5 to 6; S48. Load the resin filler in step S47 into a column.
Citation Information
Patent Citations
Extraction technology of total alkaloids of sophora alopecuroides
CN101912438A