CN101337960A - Process for extracting matrine form Chinese traditional medicine extract - Google Patents
Process for extracting matrine form Chinese traditional medicine extract Download PDFInfo
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- CN101337960A CN101337960A CNA2008101507535A CN200810150753A CN101337960A CN 101337960 A CN101337960 A CN 101337960A CN A2008101507535 A CNA2008101507535 A CN A2008101507535A CN 200810150753 A CN200810150753 A CN 200810150753A CN 101337960 A CN101337960 A CN 101337960A
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- molecularly imprinted
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Abstract
The invention discloses a method for extracting matrine from a sophora flavescens ait, which comprises three steps as follows: matrine molecular imprinting polymer is prepared, matrine molecular imprinting polymer is used as solid-phase extraction medium, and a matrine molecular imprinting solid-phase extraction column is used for extracting and separating matrine. A novel continuous rodlike molecule imprinting polymer which is synthesized by taking matrine as template molecules has the specific capacity for recognizing matrine; obtained polymer is prepared into the solid-phase extraction column through the means of packing or direct synthesis in the column; the method can be used for extraction, separation and purification of matrine; the obtained product has high purity quotient, the operating procedure is simple, the solvent usage is reduced, the extraction is safer and environment-friendly, and the purposes of removing impurities as well as purifying and enriching matrine can be served.
Description
Technical field
The invention belongs to medical processing field, relate to a kind of method of extracting matrine, especially a kind of method of from kuh-seng, extracting matrine.
Background technology
The matrine extractive technique has at present:
(1) solvent-extraction process.As decocting method, pickling process, percolation etc.
(2) ion exchange method.Utilize alkaloid salt to pass through the strongly acidic cation-exchange post, make the alkaloid salt cationic exchange on resin, but not alkaloid compound then flows out outside the post, the resin after the exchange is dried,, adopt the principle of chloroform extraction with the ammoniacal liquor alkalization.Its technological line is: kuh-seng powder → methanol eddy extraction → recovery solvent → crude extract → dilute sulphuric acid dissolving → degreasing → water layer → and except that tanning → go up D201 type Zeo-karb → alkalization resin → chloroform extraction → recovery solvent → dehydration → acetone → matrine crystallization.
(3) supercritical CO
2The fluid extraction method.
In the matrine extracting method of the above prior art, solvent-extraction process exists that loss of effective components is big, the cycle is long, many, the not high shortcoming of extraction yield of operation.Ion exchange method, the process complexity, complex operation, extraction are lost big, and production efficiency is low, and consumption of organic solvent is big, contaminate environment.Supercritical CO
2The fluid extraction method is extracted the alkaloids composition is difficult, and extraction yield is lower.
Summary of the invention
The objective of the invention is to overcome the shortcoming of above-mentioned prior art, a kind of method of extracting matrine from kuh-seng is provided, changing the method for extracting matrine and be with the matrine molecularly imprinted polymer is the Solid-Phase Extraction medium, and it has the specific recognition ability to matrine.This method has simple, the advantages such as the solvent usage quantity is little, quick, effective, environmental protection of process.
The objective of the invention is to solve by the following technical programs:
This method of extracting matrine from kuh-seng is characterized in that may further comprise the steps:
(1) preparation of matrine molecularly imprinted polymer:
A) at first in test tube, add 1～5% template molecule matrine, 2～7% function monomer, 20～60% linking agent, 30～70% pore-creating agent and 0.01～1% initiator successively according to weight ratio, vortex 0.5～60min, ultrasonic 0.5～60min make it become the homogeneous system; Described function monomer is one or more mixtures in vinylformic acid, methacrylic acid, trifluoromethyl acrylate, vinyl benzoic acid, methylene-succinic acid, 2-acrylamide-2-methyl isophthalic acid-propanesulfonic acid, vinyl pyridine, vinyl imidazole, methyl methacrylate, hydroxyethyl methylacrylate and acrylamide and N-(4-ethylene benzyl) the iminodiethanoic acid ketone; Described linking agent is one or more mixtures in ethylene glycol dimethacrylate, trimethoxy propane trimethyl acrylic ester and the pentaerythritol triacrylate; Described pore-creating agent is one or more mixtures in toluene-lauryl alcohol system, normal hexane-lauryl alcohol system and the chloroform-lauryl alcohol system; Described initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile);
B) to behind the logical nitrogen of the above-mentioned solution that mixes, it is added in stainless steel column jecket, with the sealed at both ends and vertical placement of stainless steel column jecket, at 10～100 ℃ of following isothermal reaction 1～100h;
C) after above-mentioned reaction finishes, remove seal head it is received on the liquid chromatography pump, flushing goes the template molecule matrine to obtain the matrine molecularly imprinted polymer;
(2) be the Solid-Phase Extraction medium with the matrine molecularly imprinted polymer:
The matrine molecularly imprinted polymer of removing template molecule is got from stainless steel tube, oven dry, grind, sieve, get the particle that particle diameter is 25～40 μ m, join in the methyl alcohol, make it fully dissolve formation homogenate, then homogenate is packed in the polypropylene post, under condition of negative pressure, with obtaining the matrine molecularly imprinted solid phase extraction column after the washed with methanol.
(3) the matrine molecularly imprinted solid phase extraction column is to the extraction separation of matrine:
Get kuh-seng medicinal material fine powder and add alcohol reflux, concentrated extracting solution, after enriched material water dissolution, the filtration, be loaded on the matrine molecularly imprinted solid phase extraction column of preparation, load the matrine molecularly imprinted solid phase extraction column of extracting solution with washed with methanol, used methyl alcohol-this matrine molecularly imprinted solid phase extraction column of Glacial acetic acid liquid wash-out again, collected elutriant, and be concentrated into driedly, obtain matrine.
The weight ratio of above-mentioned template molecule matrine, function monomer, linking agent, pore-creating agent and initiator is preferably 3.1%: 4.4%: 29.3%: 62.8%: 0.4%.
Above-mentioned methyl alcohol-Glacial acetic acid liquid is the mixed solution of methyl alcohol and Glacial acetic acid, and wherein the volume ratio of methyl alcohol and Glacial acetic acid is 4: 1.
The present invention is that this new continuous rodlike molecule of template molecule synthetic imprinted polymer has the specific recognition ability to matrine with the matrine, with resulting polymers with load or directly in post the synthetic mode be prepared into solid-phase extraction column, the extraction separation, the purifying that can be used for matrine, products obtained therefrom purity height, operating process is simple, reduced the solvent usage quantity, extract safer, environmental protection, can reach the purpose of removing impurity, purifying and enrichment matrine.
Description of drawings
Fig. 1 is the electron-microscope scanning figure of synthetic matrine molecularly imprinted polymer of the present invention.
Embodiment
Below in conjunction with embodiment the present invention is done and to describe in further detail:
Embodiment 1
1) the matrine molecularly imprinted polymer is synthetic:
Take by weighing mass percent than the Diisopropyl azodicarboxylate (AIBN) of the template molecule matrine that is 3.1%, 4.4% vinylformic acid, 29.3% ethylene glycol dimethacrylate (EDMA), toluene-lauryl alcohol system (being the mixture of toluene and 12 systems) of 62.8% and 0.4% 3g altogether, vortex 20min, ultrasonic 20min make it become the homogeneous system.Logical an amount of nitrogen adds this solution in the stainless steel column jecket after making solution and nitrogen can fully contacting, and is sealed at both ends, vertically places, at 50 ℃ of following isothermal reaction 40h.Reaction is removed seal head it is received on the liquid chromatography pump after finishing, and usefulness methyl alcohol-acetic acid (4: 1, V/V) as moving phase, with 0.5mlmin
-1Flow velocity washes to baseline values, and the continuous rodlike polymer material of gained white is the matrine molecularly imprinted polymer in the stainless pipe.
2) the matrine molecularly imprinted solid phase extraction column is synthetic:
The matrine molecularly imprinted polymer of removing template molecule is got from stainless steel tube, oven dry (general dry getting final product), grind, sieve, get the particle that particle diameter is 25～40 μ m, take by weighing 1.5～2g, be added to homogenate in the methyl alcohol, in the polypropylene post of packing into, under condition of negative pressure, use washed with methanol, promptly get the matrine molecularly imprinted solid phase extraction column.
3) matrine molecule solid-phase extraction column is used for the extraction of matrine:
Take by weighing kuh-seng medicinal material fine powder 5g, 60% alcohol reflux of adding 100ml three times, each 2h, concentrated extracting solution, water bath method in furnace pot.The enriched material water dissolution is filtered, and promptly gets the kuh-seng reflux extracting liquid;
The matrine molecularly imprinted solid phase extraction column is received on the liquid phase, and (4: 1, V/V) liquid fully washes, and was extremely neutral with washed with methanol again with methyl alcohol-Glacial acetic acid.Get kuh-seng reflux extracting liquid 20 μ l, the sampler by liquid phase is loaded on the solid-phase extraction column, and water is with 0.5mlmin
-1Flow velocity flushing loaded the solid-phase extraction column 20 minutes of sample; Use again methyl alcohol-Glacial acetic acid (4: 1, V/V) with 0.5mlmin
-1Flow velocity wash-out solid-phase extraction column 20 minutes, collect elutriant.Elutriant water-bath nitrogen is blown to doing, obtain the higher matrine of purity.
Embodiment 2
1) takes by weighing 2,2'-Azobis(2,4-dimethylvaleronitrile) totally 6～12g that weight ratio is 4% template molecule matrine, 6% methacrylic acid (MAA), 20% trimethoxy propane trimethyl acrylic ester (TRIM), normal hexane-lauryl alcohol system (being the mixture of normal hexane and lauryl alcohol) of 69% and 1%, vortex 15min, ultrasonic 3min, make into a homogeneous system, behind the logical nitrogen 15min deoxygenation, this solution is packed in the stainless steel column jecket, should prevent the bubble of packing in the dress post process, after having adorned that column jecket is sealed at both ends, vertically place isothermal reaction 24h.Reaction is removed seal head after finishing, and under condition of negative pressure, (4: 1, V/V) template molecule was removed in the liquid flushing with a large amount of methyl alcohol-acetic acid with pillar.
2) the matrine molecularly imprinted polymer that will remove template molecule is got from stainless steel tube, oven dry, grind, sieve, get the particle that particle diameter is 25～40 μ m, take by weighing 3～6g, be added to homogenate in the methyl alcohol, in the polypropylene post of packing into, under condition of negative pressure, use washed with methanol, promptly get the matrine molecularly imprinted solid phase extraction column.
3) matrine molecule solid-phase extraction column is used for the extraction of matrine:
Take by weighing kuh-seng medicinal material fine powder 5g, 60% alcohol reflux of adding 100ml three times, each 2h, concentrated extracting solution, water bath method in furnace pot.The enriched material water dissolution is filtered, and promptly gets the kuh-seng reflux extracting liquid;
The matrine molecularly imprinted solid phase extraction column is received on the liquid phase, and (4: 1, V/V) liquid fully washes, and was extremely neutral with washed with methanol again with methyl alcohol-Glacial acetic acid.Get kuh-seng reflux extracting liquid 20 μ l, the sampler by liquid phase is loaded on the solid-phase extraction column, and water is with 0.5mlmin
-1Flow velocity flushing loaded the solid-phase extraction column 20 minutes of sample; Use again methyl alcohol-Glacial acetic acid (4: 1, V/V) with 0.5mlmin
-1Flow velocity wash-out solid-phase extraction column 20 minutes, collect elutriant.Elutriant water-bath nitrogen is blown to doing, obtain the higher matrine of purity.
Embodiment 3
1) takes by weighing the Diisopropyl azodicarboxylate 9g altogether that weight ratio is 3% template molecule matrine, 5% vinyl benzoic acid, 27% ethylene glycol dimethacrylate, chloroform-lauryl alcohol system of 64% and 1%, vortex 15min, ultrasonic 3min, make into a homogeneous system, behind the logical nitrogen 15min deoxygenation, this solution is packed in the stainless steel column jecket, should prevent the bubble of packing in the dress post process, after having adorned that column jecket is sealed at both ends, vertically place isothermal reaction 24h.Reaction is removed seal head after finishing, and under condition of negative pressure, (4: 1, V/V) template molecule was removed in the liquid flushing with a large amount of methyl alcohol-acetic acid with pillar.
2) the matrine molecularly imprinted polymer that will remove template molecule is got from stainless steel tube, oven dry, grind, sieve, get the particle that particle diameter is 25～40 μ m, take by weighing 4g, be added to homogenate in the methyl alcohol, in the polypropylene post of packing into, under condition of negative pressure, use washed with methanol, promptly get the matrine molecularly imprinted solid phase extraction column.
3) matrine molecule solid-phase extraction column is used for the extraction of matrine:
Take by weighing kuh-seng medicinal material fine powder 10g, 60% alcohol reflux of adding 100ml three times, each 2h, concentrated extracting solution, water bath method in furnace pot.The enriched material water dissolution is filtered, and promptly gets the kuh-seng reflux extracting liquid;
The matrine molecularly imprinted solid phase extraction column is received on the liquid phase, and (4: 1, V/V) liquid fully washes, and was extremely neutral with washed with methanol again with methyl alcohol-Glacial acetic acid.Get kuh-seng reflux extracting liquid 20 μ l, the sampler by liquid phase is loaded on the solid-phase extraction column, and water is with 0.5mlmin
-1Flow velocity flushing loaded the solid-phase extraction column 20 minutes of sample; Use again methyl alcohol-Glacial acetic acid (4: 1, V/V) with 0.5mlmin
-1Flow velocity wash-out solid-phase extraction column 20 minutes, collect elutriant.Elutriant water-bath nitrogen is blown to doing, obtain the higher matrine of purity.
Embodiment 4
1) the matrine molecularly imprinted polymer is synthetic:
The Diisopropyl azodicarboxylate (AIBN) that takes by weighing weight ratio and be 3.1% template molecule matrine, 4.4% methacrylic acid, 29.3% ethylene glycol dimethacrylate (EDMA), toluene-lauryl alcohol system of 62.8% and 0.4% is 18g altogether, vortex 20min, ultrasonic 20min make it become the homogeneous system.Behind the logical nitrogen this solution is added in the stainless steel column jecket, sealed at both ends, vertically place, at 50 ℃ of following isothermal reaction 40h.Reaction is removed seal head it is received on the liquid chromatography pump after finishing, and usefulness methyl alcohol-acetic acid (4: 1, V/V) as moving phase, with 0.5mlmin
-1Flow velocity washes to baseline values, and the continuous rodlike polymer material of gained white is the matrine molecularly imprinted polymer in the stainless pipe.
2) the matrine molecularly imprinted solid phase extraction column is synthetic:
The matrine molecularly imprinted polymer of removing template molecule is got from stainless steel tube, oven dry, grind, sieve, get the particle that particle diameter is 25～40 μ m, take by weighing 6～8g, be added to homogenate in the methyl alcohol, in the polypropylene post of packing into, under condition of negative pressure, use washed with methanol, promptly get the matrine molecularly imprinted solid phase extraction column.
3) matrine molecule solid-phase extraction column is used for the extraction of matrine:
Take by weighing kuh-seng medicinal material fine powder 25g, 60% alcohol reflux of adding 400ml three times, each 2h, concentrated extracting solution, water bath method in furnace pot.The enriched material water dissolution is filtered, and promptly gets the kuh-seng reflux extracting liquid;
The matrine molecularly imprinted solid phase extraction column is received on the liquid phase, and (4: 1, V/V) liquid fully washes, and was extremely neutral with washed with methanol again with methyl alcohol-Glacial acetic acid.Get kuh-seng reflux extracting liquid 20 μ l, the sampler by liquid phase is loaded on the solid-phase extraction column, and water is with 0.5mlmin
-1Flow velocity flushing loaded the solid-phase extraction column 20 minutes of sample; Use again methyl alcohol-Glacial acetic acid (4: 1, V/V) with 0.5mlmin
-1Flow velocity wash-out solid-phase extraction column 20 minutes, collect elutriant.Elutriant water-bath nitrogen is blown to doing, obtain the higher matrine of purity.
Claims (3)
1. method of extracting matrine from kuh-seng is characterized in that may further comprise the steps:
(1) preparation of matrine molecularly imprinted polymer:
A) at first in test tube, add 1～5% template molecule matrine, 2～7% function monomer, 20～60% linking agent, 30～70% pore-creating agent and 0.01～1% initiator successively according to mass percent, vortex 0.5～60min, ultrasonic 0.5～60min make it become the homogeneous system; Described function monomer is one or more mixtures in vinylformic acid, methacrylic acid, trifluoromethyl acrylate, vinyl benzoic acid, methylene-succinic acid, 2-acrylamide-2-methyl isophthalic acid-propanesulfonic acid, vinyl pyridine, vinyl imidazole, methyl methacrylate, hydroxyethyl methylacrylate and acrylamide and N-(4-ethylene benzyl) the iminodiethanoic acid ketone; Described linking agent is one or more mixtures in ethylene glycol dimethacrylate, trimethoxy propane trimethyl acrylic ester and the pentaerythritol triacrylate; Described pore-creating agent is one or more mixtures in toluene-lauryl alcohol system, normal hexane-lauryl alcohol system and the chloroform-lauryl alcohol system; Described initiator is Diisopropyl azodicarboxylate or 2,2'-Azobis(2,4-dimethylvaleronitrile);
B) to behind the logical nitrogen of the above-mentioned solution that mixes, it is added in stainless steel column jecket, with the sealed at both ends and vertical placement of stainless steel column jecket, at 10～100 ℃ of following isothermal reaction 1～100h;
C) after above-mentioned reaction finishes, remove seal head it is received on the liquid chromatography pump, flushing goes the template molecule matrine to obtain the matrine molecularly imprinted polymer;
(2) be the Solid-Phase Extraction medium with the matrine molecularly imprinted polymer:
The matrine molecularly imprinted polymer of removing template molecule is taken out from stainless steel tube, oven dry, grind, sieve, get the particle that particle diameter is 25～40 μ m, join in the methyl alcohol, make it fully dissolve formation homogenate, then homogenate is packed in the polypropylene post, under condition of negative pressure, with obtaining the matrine molecularly imprinted solid phase extraction column after the washed with methanol.
(3) the matrine molecularly imprinted solid phase extraction column is to the extraction separation of matrine:
Get kuh-seng medicinal material fine powder and add alcohol reflux, concentrated extracting solution, after enriched material water dissolution, the filtration, be loaded on the matrine molecularly imprinted solid phase extraction column of preparation, load the matrine molecularly imprinted solid phase extraction column of extracting solution with washed with methanol, used methyl alcohol-this matrine molecularly imprinted solid phase extraction column of Glacial acetic acid liquid wash-out again, collected elutriant, and be concentrated into driedly, obtain matrine.
2. a kind of method of extracting matrine from kuh-seng according to claim 1, it is characterized in that: the mass ratio of described template molecule matrine, function monomer, linking agent, pore-creating agent and initiator is 3.1: 4.4: 29.3: 62.8: 0.4.
3. a kind of method of from kuh-seng, extracting matrine according to claim 1, it is characterized in that: described methyl alcohol-Glacial acetic acid liquid is the mixed solution of methyl alcohol and Glacial acetic acid, wherein the volume ratio of methyl alcohol and Glacial acetic acid is 4: 1.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544626B (en) * | 2009-03-20 | 2011-08-31 | 西安交通大学 | Method for extracting genistein from plant nepeta japonica maxim |
| CN103641949A (en) * | 2013-12-16 | 2014-03-19 | 广西大学 | Molecularly imprinted material for matrine separation and purification and preparation method thereof |
| CN103664942A (en) * | 2013-12-16 | 2014-03-26 | 广西大学 | Method for extracting matrine by coupling molecular imprinting with ultrasonic extraction |
| CN103739602A (en) * | 2013-12-16 | 2014-04-23 | 广西大学 | Method for extracting matrine |
| CN104888740A (en) * | 2015-06-11 | 2015-09-09 | 大理州质量技术监督综合检测中心 | Preparation method and application of solid phase extraction column of urotropin molecular imprinting |
| CN106279488B (en) * | 2016-08-15 | 2018-05-01 | 西藏自治区农牧科学院 | The preparation for the molecularly imprinted polymer that three kinds of alkaloids of sandliving sophora seed extract at the same time and extracting process |
| CN107987079A (en) * | 2017-10-10 | 2018-05-04 | 仲恺农业工程学院 | Matrine and oxymatrine method for extraction and purification in kuh-seng |
| CN112174963A (en) * | 2020-10-13 | 2021-01-05 | 石家庄正道动物药业有限公司 | A method for processing matrine |
-
2008
- 2008-08-29 CN CNA2008101507535A patent/CN101337960A/en active Pending
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101544626B (en) * | 2009-03-20 | 2011-08-31 | 西安交通大学 | Method for extracting genistein from plant nepeta japonica maxim |
| CN103641949A (en) * | 2013-12-16 | 2014-03-19 | 广西大学 | Molecularly imprinted material for matrine separation and purification and preparation method thereof |
| CN103664942A (en) * | 2013-12-16 | 2014-03-26 | 广西大学 | Method for extracting matrine by coupling molecular imprinting with ultrasonic extraction |
| CN103739602A (en) * | 2013-12-16 | 2014-04-23 | 广西大学 | Method for extracting matrine |
| CN103641949B (en) * | 2013-12-16 | 2015-06-03 | 广西大学 | Molecularly imprinted material for matrine separation and purification and preparation method thereof |
| CN103664942B (en) * | 2013-12-16 | 2015-10-21 | 广西大学 | A kind of molecular imprinting and ultrasonic coupling extract the method for matrine |
| CN104888740A (en) * | 2015-06-11 | 2015-09-09 | 大理州质量技术监督综合检测中心 | Preparation method and application of solid phase extraction column of urotropin molecular imprinting |
| CN106279488B (en) * | 2016-08-15 | 2018-05-01 | 西藏自治区农牧科学院 | The preparation for the molecularly imprinted polymer that three kinds of alkaloids of sandliving sophora seed extract at the same time and extracting process |
| CN107987079A (en) * | 2017-10-10 | 2018-05-04 | 仲恺农业工程学院 | Matrine and oxymatrine method for extraction and purification in kuh-seng |
| CN112174963A (en) * | 2020-10-13 | 2021-01-05 | 石家庄正道动物药业有限公司 | A method for processing matrine |
| CN112174963B (en) * | 2020-10-13 | 2022-02-01 | 石家庄正道动物药业有限公司 | A method for processing matrine |
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