CN111777610A - Method for separating and purifying oxymatrine from sophora moorcroftiana extract - Google Patents
Method for separating and purifying oxymatrine from sophora moorcroftiana extract Download PDFInfo
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Abstract
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract relates to the technical field of oxymatrine purification, and comprises the following steps: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water is 1:2-4 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2-6 hours to obtain a mixed solution A; cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B; adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.2-0.6 according to the volume parts to obtain a mixed solution B; adding the mixed solution B into a certain volume of mixed solvent B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1-2 according to the volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate; filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine. The solvent has low harm to personnel, can be recycled and reused, and does not cause pollution.
Description
Technical Field
The invention relates to the technical field of oxymatrine purification, in particular to a method for separating and purifying oxymatrine from sophora moorcroftiana extract.
Background
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.
Oxymatrine is widely used in the fields of pharmacy and pesticides. Can be used for treating chronic hepatitis B, tumor radiotherapy, leucopenia caused by chemotherapy, and leukopenia caused by other reasons. The oxymatrine is natural plant pesticide, has low toxicity to human and livestock, is a broad-spectrum pesticide, and has contact poisoning and stomach poisoning effects. Has obvious control effect on armyworm, cabbage caterpillar, aphid and red spider on various crops.
The purity of the existing oxymatrine can only reach 98 percent generally, and the purity needs to be further improved, and the existing purification methods comprise an ion exchange method and a silica gel column chromatography, but the ion exchange method and the silica gel column chromatography have some problems in purifying oxymatrine, such as: high process cost, limited equipment life and industrial solid waste generated in the later period, thus being not beneficial to large-scale industrial production.
Disclosure of Invention
The invention aims to solve the technical problems and provides a method for separating and purifying oxymatrine from sophora moorcroftianain extract, which solves the defects that the traditional extraction method is not easy to transport and is not beneficial to environmental protection.
The invention is realized by the following technical scheme: a method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:2-4 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2-6 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.2-0.6 according to volume parts to obtain a mixed solution B, and the mixed solvent A consists of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1-2 according to the volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, n-hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Further, in the raw material dissolving step, the ratio of the sophora moorcroftianain extract to the 10% ammonia water is 1:3 in parts by volume, the mixture is heated to 20-80 ℃ after being mixed, and then the mixture is stirred for 2.5 hours.
Further, in the solvent mixing step, the ratio of the filtrate B to the mixed solvent A is 1:0.5 in parts by volume.
Further, in the liquid separation step, the ratio of the mixed liquid B to the mixed solvent B is 1:1.5 in parts by volume.
Compared with the prior art, the invention has the following advantages and beneficial effects: the whole separation and purification process is a solvent method, the used solvent has low harm to personnel, can be recycled, cannot cause pollution, and is suitable for large-scale industrial production; the purity of the oxymatrine purified by the separation and purification process reaches more than 99 percent, and the purification effect is good.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to examples, and the exemplary embodiments and descriptions thereof are only used for explaining the present invention and are not used as limitations of the present invention.
Example 1
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:2 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.2 according to volume parts, so as to obtain a mixed solution B, and the mixed solvent A is composed of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, normal hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Example 2
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:4 according to volume parts, mixing, heating to 20-80 ℃, and stirring for 2 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.2 according to volume parts, so as to obtain a mixed solution B, and the mixed solvent A is composed of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, normal hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Example 3
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, mixing the sophora moorcroftianain extract and the 10% ammonia water with a ratio of 1:3, heating to 20-80 ℃, and stirring for 2 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.2 according to volume parts, so as to obtain a mixed solution B, and the mixed solvent A is composed of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, normal hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Example 4
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, mixing the sophora moorcroftianain extract and the 10% ammonia water with a ratio of 1:3, heating to 20-80 ℃, and stirring for 6 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.2 according to volume parts, so as to obtain a mixed solution B, and the mixed solvent A is composed of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, normal hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Example 5
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:3 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2.5 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.2 according to volume parts, so as to obtain a mixed solution B, and the mixed solvent A is composed of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B is petroleum ether, n-hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Example 6
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:3 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2.5 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.6 according to volume parts to obtain a mixed solution B, and the mixed solvent A consists of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, normal hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Example 7
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:3 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2.5 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.5 according to volume parts, so as to obtain a mixed solution B, and the mixed solvent A consists of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, normal hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Example 8
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:3 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2.5 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.5 according to volume parts, so as to obtain a mixed solution B, and the mixed solvent A consists of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:2 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, normal hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Example 9
A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract comprises the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:3 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2.5 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.5 according to volume parts, so as to obtain a mixed solution B, and the mixed solvent A consists of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1.5 according to volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, n-hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
Examples of the experiments
The oxymatrine purity of examples 1-9 was tested under otherwise constant conditions using existing test methods, such as TLC methods, with the following results:
according to the results of the experimental examples, the process parameters used in example 9 were optimized in consideration of the consumption of raw materials and the purification effect. In addition, compared with the traditional purification method, the purification method of the invention can obtain good purification effect.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only illustrative of the present invention and are not intended to limit the scope of the present invention, and any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (4)
1. A method for separating and purifying oxymatrine from Sophora Moorcroftiana extract is characterized by comprising the following steps:
raw material dissolution: adding 10% ammonia water with a certain volume concentration into the sophora moorcroftianain extract, wherein the ratio of the sophora moorcroftianain extract to the 10% ammonia water with the concentration is 1:2-4 in parts by volume, mixing, heating to 20-80 ℃, and stirring for 2-6 hours to obtain a mixed solution A;
cooling and filtering: cooling the mixed solution A, and filtering to remove insoluble substances to obtain a filtrate B;
mixing the solvents: adding a certain volume of mixed solvent A into the filtrate B, wherein the ratio of the filtrate B to the mixed solvent A is 1:0.2-0.6 according to volume parts to obtain a mixed solution B, and the mixed solvent A consists of ethyl acetate, petroleum ether, methanol, ethanol, n-butanol and/or isopropanol;
liquid separation: adding a certain volume of mixed solvent B into the mixed solution B, wherein the ratio of the mixed solution B to the mixed solvent B is 1:1-2 according to the volume parts, and then carrying out liquid separation through a liquid separator to obtain a precipitate, wherein the mixed solvent B consists of petroleum ether, n-hexane and/or diethyl ether;
and (3) filtering and drying: filtering the precipitate, and vacuum drying for 1-2 hr to obtain purified oxymatrine.
2. The method for separating and purifying oxymatrine from Sophora moorcroftiana extract as claimed in claim 1, wherein in the raw material dissolving step, the ratio of the Sophora moorcroftiana extract to the 10% ammonia water is 1:3 by volume, and after mixing, heating to 20-80 ℃, and then stirring for 2.5 hours.
3. The method for separating and purifying oxymatrine from Sophora moorcroftiana extract as claimed in claim 2, wherein in the solvent mixing step, the ratio of the filtrate B to the mixed solvent A is 1:0.5 in parts by volume.
4. The method for separating and purifying oxymatrine from Sophora moorcroftiana extract as claimed in claim 3, wherein in the step of separating, the ratio of the mixed solution B to the mixed solvent B is 1:1.5 by volume.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1793143A (en) * | 2005-12-27 | 2006-06-28 | 中国科学院山西煤炭化学研究所 | Process for producing high purity matrine oxide |
| CN1793142A (en) * | 2005-12-27 | 2006-06-28 | 中国科学院山西煤炭化学研究所 | Process for producing high purity matrine oxide by kuh-seng |
| CN1978446A (en) * | 2005-11-29 | 2007-06-13 | 中国科学院地理科学与资源研究所 | Process for extracting oxymatrine and matrine from sophora moocroftiana |
| CN102766143A (en) * | 2012-07-30 | 2012-11-07 | 安徽省科学技术研究院 | Method for extracting oxymatrine from Sophora moorcroftiana seeds |
-
2020
- 2020-07-31 CN CN202010760535.4A patent/CN111777610A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1978446A (en) * | 2005-11-29 | 2007-06-13 | 中国科学院地理科学与资源研究所 | Process for extracting oxymatrine and matrine from sophora moocroftiana |
| CN1793143A (en) * | 2005-12-27 | 2006-06-28 | 中国科学院山西煤炭化学研究所 | Process for producing high purity matrine oxide |
| CN1793142A (en) * | 2005-12-27 | 2006-06-28 | 中国科学院山西煤炭化学研究所 | Process for producing high purity matrine oxide by kuh-seng |
| CN102766143A (en) * | 2012-07-30 | 2012-11-07 | 安徽省科学技术研究院 | Method for extracting oxymatrine from Sophora moorcroftiana seeds |
Non-Patent Citations (1)
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Application publication date: 20201016 |