CN111349097A - Preparation method of matrine - Google Patents
Preparation method of matrine Download PDFInfo
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- CN111349097A CN111349097A CN201811565883.5A CN201811565883A CN111349097A CN 111349097 A CN111349097 A CN 111349097A CN 201811565883 A CN201811565883 A CN 201811565883A CN 111349097 A CN111349097 A CN 111349097A
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- matrine
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/22—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed systems contains four or more hetero rings
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Abstract
The invention discloses a preparation method of matrine, which comprises the following steps: pulverizing radix Sophorae Alopecuroidis, adding ethanol, soaking, and extracting with ultrasonic for 2 times to obtain ethanol extract of Sophora Alopecuroidis matrine; vacuum concentrating the above ethanol extractive solution to obtain matrine crude extract. Adding acetone solution into the matrine crude extract, and extracting for 2 times by ultrasonic method to obtain acetone extract of Sophora alopecuroides matrine; adding diatomite into the acetone extracting solution, stirring and decoloring, and filtering to obtain a decoloring solution; separating and purifying the matrine decolorized solution by ion exchange chromatography; vacuum concentrating the purified matrine solution, and crystallizing with methanol to obtain refined matrine. The method provided by the invention adopts an ultrasonic method to be matched with ethanol and acetone for two times of extraction, so that the cell wall structure of the sophora alopecuroides is fully destroyed, most of matrine in the cells of the sophora alopecuroides can be released, the yield of the matrine is higher, and the purity of the matrine is greatly improved.
Description
Technical Field
The invention relates to the technical field of biological medicine preparation, and in particular relates to a preparation method of matrine.
Background
Sophora alopecuroides root, root of Sophora alopecuroides L of Leguminosae. Distributed in North China, northwest China, Henan and Tibet. Has effects of clearing intestine, eliminating dampness, and relieving pain. It is commonly used for damp-heat dysentery, enteritis and diarrhea, jaundice, eczema, pharyngalgia, toothache, intractable tinea, and scald. Matrine is prepared from dried root, plant and fruit of Sophora flavescens ait of Leguminosae by extracting with organic solvent such as ethanol, and is an alkaloid. The matrine is a general term of all alkaloids of radix sophorae flavescentis (the detection method of the matrine is a titration method), and the main components of the matrine comprise various alkaloids such as matrine, sophocarpine, oxysophocarpine and sophoridine, and the content of the matrine and the oxysophocarpine is the highest. Other sources are Sophora alopecuroides fruit, Sophora subprostrata and the overground part of the Sophora subprostrata, and the pure product is off-white to white powder in appearance.
In the prior art, the extraction method of matrine is generally single ethanol soaking and heating extraction, and finally the obtained extracting solution is centrifuged to take supernatant as the matrine obtained by extraction. However, the extraction process of the matrine is simple, and the extracted matrine has low purity.
Disclosure of Invention
The invention aims to solve the technical problem of providing matrine and a preparation method thereof.
The technical scheme adopted by the invention for solving the technical problems is as follows:
a preparation method of matrine comprises the following steps:
(1) taking a certain amount of sophora alopecuroide, and crushing the sophora alopecuroide in a crusher;
(2) adding 10-20 times of 60-75% ethanol by weight into the sophora alopecuroide powder in the step (1), soaking for 30-60 minutes, extracting for 2 times by matching an ultrasonic method, each time for 1-3 hours, combining the two extracting solutions, and standing to obtain an ethanol extracting solution of sophora alopecuroide matrine;
(3) and (3) concentrating the first ethanol extracting solution obtained in the step (2) in vacuum to obtain an extract to obtain a matrine crude extract.
(4) Adding 10-20 times of 50-60% acetone solution into the matrine crude extract obtained in step (3), extracting for 2 times by ultrasonic method, each time for 1-3 hr, mixing the two extractive solutions, and standing to obtain acetone extractive solution of Sophora alopecuroides matrine;
(5) adding 1-2% of diatomite by mass into the acetone extracting solution obtained in the step (4), stirring and decoloring for 2 hours, and filtering to obtain a decoloring solution;
(6) separating and purifying the matrine decolorized solution in the step (5) by adopting an ion exchange chromatography, and collecting a purified matrine solution;
(7) vacuum concentrating the purified matrine solution, and crystallizing with methanol to obtain refined matrine;
in a further technical scheme, the ultrasonic extraction conditions of the step (2) are as follows: the ultrasonic frequency is 70-120 Hz, and the temperature is 60-80 ℃.
In a further technical scheme, the ultrasonic extraction conditions of the step (4) are as follows: the ultrasonic frequency is 90-150 Hz, and the temperature is 50-60 ℃. Compared with the prior art, the invention has the following beneficial effects:
according to the method provided by the invention, the cell wall structure of the sophora alopecuroides is damaged by combining a conventional ethanol extraction method with an ultrasonic extraction method, most of matrine in cells of the sophora alopecuroides can be released, the yield is higher than that of direct extraction, and the acetone fine extraction is carried out for the second time on the basis, so that the purity of the matrine is greatly improved;
Detailed Description
For a better understanding of the present invention, reference is made to the following examples. It is to be understood that these examples are for further illustration of the invention and are not intended to limit the scope of the invention. In addition, it should be understood that the invention is not limited to the above-described embodiments, but is capable of various modifications and changes within the scope of the invention.
Example 1
Taking a certain amount of sophora alopecuroide, and crushing the sophora alopecuroide in a crusher; adding 15 times of 70% ethanol by weight into the sophora alopecuroide powder, soaking for 45 minutes, then extracting for 2 times by an ultrasonic method under the conditions that the ultrasonic frequency is 70-120 Hz and the temperature is 75 ℃ and each time is 2 hours, combining the two extracting solutions, and standing to obtain the sophora alopecuroide matrine ethanol extracting solution; vacuum concentrating the first ethanol extractive solution to obtain extract to obtain matrine crude extract. Adding 10 times of 55% acetone solution into the obtained matrine crude extract, extracting for 2 times by ultrasonic method under the conditions of ultrasonic frequency of 90-150 Hz and temperature of 50-60 ℃ for 3 hours each time, combining the two extracting solutions, and standing to obtain acetone extracting solution of sophora alopecuroide matrine; adding 1% of diatomite by mass into the obtained acetone extracting solution, stirring and decoloring for 2 hours, and filtering to obtain a decoloring solution; separating and purifying the matrine decolorized solution in the above step by ion exchange chromatography, and collecting purified matrine solution; vacuum concentrating the purified matrine solution, and crystallizing with methanol to obtain refined matrine.
Example 2
Taking a certain amount of sophora alopecuroide, and crushing the sophora alopecuroide in a crusher; adding 20 times of 65% ethanol by weight into the sophora alopecuroide powder, soaking for 60 minutes, then extracting for 2 times by an ultrasonic method under the conditions that the ultrasonic frequency is 70-120 Hz and the temperature is 80 ℃ for 3 hours each time, combining the two extracting solutions, and standing to obtain the sophora alopecuroide matrine ethanol extracting solution; vacuum concentrating the first ethanol extractive solution to obtain extract to obtain matrine crude extract. Adding 15 times of 60% acetone solution into the obtained matrine crude extract, extracting for 2 times by ultrasonic method under the conditions of ultrasonic frequency of 90-150 Hz and temperature of 58 ℃ for 3 hours each time, combining the two extracting solutions, and standing to obtain acetone extracting solution of sophora alopecuroide matrine; adding 1.5% of diatomite by mass into the obtained acetone extracting solution, stirring and decoloring for 2 hours, and filtering to obtain a decoloring solution; separating and purifying the matrine decolorized solution in the above step by ion exchange chromatography, and collecting purified matrine solution; vacuum concentrating the purified matrine solution, and crystallizing with methanol to obtain refined matrine.
As described above, the present invention can be preferably implemented.
Claims (3)
1. A preparation method of matrine is characterized by comprising the following steps:
(1) pulverizing a certain amount of herba Sophorae Alopecuroidis in a pulverizer
(2) Adding 10-20 times of 60-75% ethanol by weight into the sophora alopecuroide powder in the step (1), soaking for 30-60 minutes, extracting for 2 times by matching an ultrasonic method, each time for 1-3 hours, combining the two extracting solutions, and standing to obtain an ethanol extracting solution of sophora alopecuroide matrine;
(3) and (3) concentrating the first ethanol extracting solution obtained in the step (2) in vacuum to obtain an extract to obtain a matrine crude extract.
(4) Adding 10-20 times of 50-60% acetone solution into the matrine crude extract obtained in step (3), extracting for 2 times by ultrasonic method, each time for 1-3 hr, mixing the two extractive solutions, and standing to obtain acetone extractive solution of Sophora alopecuroides matrine;
(5) adding 1-2% of diatomite by mass into the acetone extracting solution obtained in the step (4), stirring and decoloring for 2 hours, and filtering to obtain a decoloring solution;
(6) separating and purifying the matrine decolorized solution in the step (5) by adopting an ion exchange chromatography, and collecting a purified matrine solution;
(7) vacuum concentrating the purified matrine solution, and crystallizing with methanol to obtain refined matrine.
2. The method for preparing matrine according to claim 1, wherein the ultrasonic extraction conditions in step (2) are as follows: the ultrasonic frequency is 70-120 Hz, and the temperature is 60-80 ℃.
3. The method for preparing matrine according to claim 1, wherein the ultrasonic extraction conditions in step (4) are as follows: the ultrasonic frequency is 90-150 Hz, and the temperature is 50-60 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811565883.5A CN111349097A (en) | 2018-12-20 | 2018-12-20 | Preparation method of matrine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811565883.5A CN111349097A (en) | 2018-12-20 | 2018-12-20 | Preparation method of matrine |
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| CN111349097A true CN111349097A (en) | 2020-06-30 |
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| CN201811565883.5A Pending CN111349097A (en) | 2018-12-20 | 2018-12-20 | Preparation method of matrine |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115590039A (en) * | 2022-08-23 | 2023-01-13 | 尹长年（Cn） | Insecticidal composition and preparation method thereof |
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2018
- 2018-12-20 CN CN201811565883.5A patent/CN111349097A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115590039A (en) * | 2022-08-23 | 2023-01-13 | 尹长年（Cn） | Insecticidal composition and preparation method thereof |
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Application publication date: 20200630 |