CN104072496A - Preparation method for Guanfu base A and salt thereof - Google Patents
Preparation method for Guanfu base A and salt thereof Download PDFInfo
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- CN104072496A CN104072496A CN201310097092.5A CN201310097092A CN104072496A CN 104072496 A CN104072496 A CN 104072496A CN 201310097092 A CN201310097092 A CN 201310097092A CN 104072496 A CN104072496 A CN 104072496A
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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
- C07D471/02—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 system contains two hetero rings
- C07D471/10—Spiro-condensed systems
Abstract
The invention provides a preparation method for Guanfu base A and a salt thereof. According to the method, acid water extraction technology and cationic adsorption resin purifying technology are used together, organic acid precipitation is employed to remove impurities, and recrystallization is carried out so as to obtain Guanfu base A and the salt thereof. Specifically speaking, the method comprises the following steps: step 1, extracting the medicinal material--Korean monkshood root with acid water so as to obtain an extract A; step 2, purifying the extract A with cationic resin so as to obtain a purified substance; step 3, adding organic acid into the purified substance obtained in the step 2, carrying out precipitation and subjecting a precipitate to alkalization so as to obtain a crude Guanfu base A product; and step 4, subjecting the crude Guanfu base A product obtained in the step 3 to recrystallization. The method can rapidly increase the content of Guanfu base A in the product and substantially shortens a crystallization cycle.
Description
Technical field
The invention provides a kind of method of extracting separated Guan-fubase A and salt thereof from herbal medicine, be specifically related to a kind of method of extracting separated Guan-fubase A and salt thereof from Radix Aconiti Coreani.
Background technology
Typhoniun Tuber is the piece root of Chinese medicine Ranunculaceae Radix Aconiti Coreani Aconitum coreanum (L é vl.) Rapaics, is one of conventional Chinese medicine, and tcm clinical practice is used for arthralgia due to cold-dampnes by Typhoniun Tuber for many years, migraine, and waist knee joint crymodynias etc., achieve good results.Modern pharmacological research shows that in Typhoniun Tuber, main active ingredient is C
20diterpenoid Alkaloids compounds, mainly comprises Guan-fubase B (Guanfu base G, GFG), and Guan-fubase A (Guanfu base A, GFA) closes attached element in the ninth of the ten Heavenly Stems (Guanfu base I, GFI) etc.
Preclinical pharmacology research shows: Guan-fu base A hydrochloride can resist ventricular tachycardia and the ventricular fibrillation of high calcium, following coronary artery occlusion and Aconitine Induced, and can resist auricular flutter and the atrial fibrillation of Acetylcholine-induced; Can reduce the V to myocardium fast response action potential by concentration dependent
max.The full cell method of patch clamp proves that this medicine inhibition fast response myocardial cell's the interior stream of Na+ is main polyion channeling, is the natural product of a good anti-heart disorder.A large amount of clinical datas show, Guan-fu base A hydrochloride is the active drug of tachycardia and ventricular arythmia on treatment paroxysmal chamber, certainly, untoward reaction is few and slight for curative effect, is the former new medicine of anti-heart disorder Western medicine one class of safe and effective wide spectrum of the brand new type found first.
Prior art adopts the method for multistep extraction to prepare Guan-fu base A hydrochloride more, and Chinese patent CN1088827A has announced the preparation technology of Guan-fubase A, and this technique ethanol extraction yield is low, and defatting step has adopted a large amount of organic solvents, and environmental pollution is serious; Extraction step emulsification is serious, and extraction efficiency is low; Wherein use the method for column chromatography, Guan-fubase A loss is large, and equipment requirements is high, complex operation step, and Guan-fubase A yield is low; Crystallisation step carries out in the more situation of impurity, crystallization difficulty, and crystallizing cycle very long (several weeks), and also yield is lower.
Summary of the invention
The preparation method who the object of this invention is to provide a kind of Guan-fubase A.
The preparation method who the object of this invention is to provide a kind of Guan-fubase A salt.
The object of the invention is to be achieved through the following technical solutions:
Scheme one:
A preparation method for Guan-fubase A, the method comprises:
Step 1: get Typhoniun Tuber acid extraction, obtain extracting solution A;
Step 2: extracting solution A, by resin cation (R.C.) purifying, obtains purified (alkaloids substance);
Step 3: the purified that step 2 is obtained adds organic acid, precipitation, obtains throw out, after throw out is alkalized, obtains Guan-fubase A crude product;
Step 4: step 3 gained Guan-fubase A crude product carries out recrystallization.
Further, described in step 1, sour water is selected from any one in the hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid of 0.1-3%; The hydrochloric acid of preferred 0.1-3%.Sour water consumption is medicinal material: sour water (kg/L)=1:20-40.
Further, described in step 1, extracting method is selected from dipping extraction, diacolation extraction, refluxing extraction, supersound extraction any one; Preferably diacolation extracts or refluxing extraction.
Further, Zeo-karb purifying is described in step 2: step 1 extracting solution A is adsorbed in to Zeo-karb, to be exchangedly resin is taken out after completely, alkalization, with organic solvent extraction, reclaims solvent and obtain purified (alkaloids substance); Wherein, described Zeo-karb comprises and take any one strongly-acid that is framework material or weakly acidic cation-exchange resin in vinylbenzene, divinylbenzene, acrylate or methacrylic ester; Be preferably and take the storng-acid cation exchange resin that vinylbenzene is framework material; Described alkalization is selected from any one in sodium hydroxide solution, potassium hydroxide solution, strong aqua or sodium carbonate solution with solution, alkalizes to the preferred pH10-12 of pH8-12(); Described extraction is one or more the mixed solvent in chloroform, methyl alcohol, ethanol, propyl alcohol, butanols, ethyl acetate, ritalin, acetone, ether with organic solvent; Be preferably the mixing solutions of methyl alcohol and ethyl acetate; The consumption of described organic solvent is 3-6 times (v/v) of resin demand.
Further, described in step 3, organic acid is selected from any one in oxalic acid, tartrate, citric acid; Being acidified to pH is the preferred pH1-3 of 1-4().
Further, described in step 3 taking precipitate alkalize to pH be the preferred pH9-11 of 8-11().
Further, described in step 3, throw out carries out drying or cryodrying after alkalinisation treatment; Further, described cryodrying temperature is not higher than 50 ℃.
Further, described in step 4, the organic solvent of recrystallization is one or more the mixture in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol, chloroform, ethyl acetate and acetone.
Further, a kind of preparation method of Guan-fubase A, the method comprises:
Step 1: get Typhoniun Tuber medicinal material, pulverize, by sour water diacolation or refluxing extraction, obtain extracting solution A;
Step 2: the extracting solution A that step 1 is obtained is adsorbed in Zeo-karb, to be exchangedly takes out resin after completely, dry, the strong aqua of take alkalize to pH be 8-12, with organic solvent refluxing extraction, reclaim solvent and obtain purified (alkaloids substance);
Step 3: it is 1-4 to pH that the purified that step 2 is obtained adds organic acid, and precipitation, filters, taking precipitate is with water furnishing pasty state, strong aqua alkalize to pH be 8-12, dry, obtain Guan-fubase A crude product;
Step 4: the Guan-fubase A crude product that step 3 is obtained carries out recrystallization with organic solvent, filters, dry, obtains Guan-fubase A.
Scheme two:
A preparation method for Guan-fubase A salt, the method comprises:
Step 1: Typhoniun Tuber acid extraction, obtains extracting solution A;
Step 2: extracting solution A carries out purifying by resin cation (R.C.), obtains purified (alkaloids substance);
Step 3: the purified that step 2 is obtained adds organic acid, precipitation, obtains throw out, and taking precipitate carries out alkalinisation treatment and obtains Guan-fubase A crude product;
Step 4: the Guan-fubase A crude product that step 3 is obtained redissolves with organic solvent, adding acid solution to regulate pH is 1-6, standing crystallization, then with organic solvent recrystallization, obtain Guan-fubase A salt.
Further, described in step 1, sour water is selected from any one in the hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid of 0.1-3%; The hydrochloric acid of preferred 0.1-3%.Sour water consumption is medicinal material: sour water (Kg/L)=1:20-40.
Further, described in step 1, extracting method is selected from dipping extraction, diacolation extraction, refluxing extraction, supersound extraction any one; Preferably diacolation extracts or refluxing extraction.
Further, Zeo-karb purifying is described in step 2: step 1 extracting solution A is adsorbed in to Zeo-karb, to be exchangedly resin is taken out after completely, alkalization, with organic solvent extraction, reclaims solvent and obtain purified (alkaloids substance); Wherein, described Zeo-karb comprises and take any one strongly-acid that is framework material or weakly acidic cation-exchange resin in vinylbenzene, divinylbenzene, acrylate or methacrylic ester; Be preferably and take the storng-acid cation exchange resin that vinylbenzene is framework material; Described alkalization is selected from any one in sodium hydroxide solution, potassium hydroxide solution, strong aqua or sodium carbonate solution with solution, alkalizes to the preferred pH10-12 of pH8-12(); Described extraction is one or more the mixed solvent in chloroform, methyl alcohol, ethanol, propyl alcohol, butanols, ethyl acetate, ritalin, acetone, ether with organic solvent; Be preferably the mixing solutions of methyl alcohol and ethyl acetate; The consumption of described organic solvent is 3-6 times (v/v) of resin demand.
Further, described in step 3, organic acid is selected from any one in oxalic acid, tartrate, citric acid; Being acidified to pH is the preferred pH1-3 of 1-4().
Further, described in step 3 taking precipitate alkalize to pH be the preferred pH9-11 of 8-11().
Further, described in step 3, throw out carries out drying or cryodrying after alkalinisation treatment; Further, described cryodrying temperature is not higher than 50 ℃.
Further, described in step 4, the organic solvent of recrystallization is one or more the mixture in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol, chloroform, ethyl acetate and acetone.
Further, a kind of preparation method of Guan-fubase A hydrochloride, the method comprises:
Step 1: get Typhoniun Tuber medicinal material, pulverize, by sour water diacolation or refluxing extraction, obtain extracting solution A;
Step 2: the extracting solution A that step 1 is obtained is adsorbed in Zeo-karb, to be exchangedly takes out resin after completely, dry, the strong aqua of take alkalize to pH be 8-12, with organic solvent refluxing extraction, reclaim solvent and obtain purified (alkaloids substance);
Step 3: the purified that step 2 is obtained add organic acid to pH be the preferred pH1-3 of 1-4(), precipitation, filters, taking precipitate is with water furnishing pasty state, strong aqua alkalize to pH be 8-11, dry, obtain Guan-fubase A crude product;
Step 4: the Guan-fubase A crude product that step 3 is obtained redissolves with organic solvent, enriching hcl acidifying is 1-6 to pH, standing crystallization, then carry out recrystallization with organic solvent, and filter, dry, obtain Guan-fubase A hydrochloride.
In addition, the present invention also provides a kind of and has prepared Guan-fubase A product by aforesaid method.
Wherein, in this Guan-fubase A product, the content of Guan-fubase A is greater than 98%.
Technical solution of the present invention has following advantage compared to existing technology:
1, adopt acid extraction and cation-adsorption resin to purify the technique combining and extract Typhoniun Tuber total alkaloids, organic solvent extraction compared to existing technology, not only saves cost, reduces environmental pollution, and reduced the loss of target component Guan-fubase A, improved the extraction yield of Guan-fubase A.
The serious problem of emulsification while 2, having avoided extracting solution to concentrate afterwards directly with organic solvent extraction, equipment requirements is not high, and operability is very strong.
3, the purifying method that directly adds Acid precipitation after employing organic solvent extraction, the content of Guan-fubase A in Quick high product, shortens crystallizing cycle greatly.Compared with prior art, in the situation that guaranteeing Guan-fubase A purity (all reaching more than 98%) and yield (the highest yield reaches 3.16 ‰), its crystallizing cycle is only 1/10 of prior art to the inventive method.
Effect experimental example
The impact of experimental example 1 Different Extraction Method on Guan-fubase A extraction yield
1 sample preparation
Experimental group: get 1kg Typhoniun Tuber medicinal material, broken, 200L0.1% sulfuric acid diacolation extracts, extracting solution is adsorbed in 25LAmberlite IR-20 Zeo-karb, take out resin, dry, resin take strong aqua alkalize to pH be 10, resin after alkalization extracts with 100L ethyl acetate and methanol mixed solvent refluxing, reclaims solvent and obtains total alkaloids.
Control group: get 1kg Typhoniun Tuber medicinal material, pulverize ethanol percolate extraction, reclaim ethanol, obtain medicinal extract, add 1% dissolving with hydrochloric acid, acid liquid is adjusted pH3, and standing sour water liquation glue, precipitates in filtering acid liquid, with petroleum ether degreasing, minute remove petroleum ether layer, with dense ammonia alkali acid liquid to pH5, use again chloroform extraction, collect chloroform solution, reclaim under reduced pressure chloroform, obtains total alkaloids.
2 Guan-fubase A content assaying methods
The preparation of 2.1 reference substance solution:
Get Guan-fu base A hydrochloride reference substance appropriate, accurately weighed, add methyl alcohol and make every 1ml containing the solution of 0.50mg, shake up, obtain.
The preparation of 2.2 need testing solutions:
Get experimental group total alkaloids, each 10mg of control group total alkaloids fine powder, accurately weighed, put respectively in 10ml measuring bottle, add methyl alcohol supersound process and make to dissolve and be diluted to scale, shake up, filter, get subsequent filtrate, obtain.
2.3 chromatographic conditions:
With octadecylsilane chemically bonded silica, it is weighting agent; With the heptanesulfonic acid sodium water solution of 2ml/ml (containing 0.2% triethylamine, and take phosphoric acid adjust pH to 3.0)-acetonitrile (75:25), be moving phase; Detection wavelength is 205nm.
3 experimental results
Employing marker method is carried out, and measurement result is in Table 1.
The comparison of table 1 Different Extraction Method Guan-fubase A content
| ? | Experimental group | Control group |
| Guan-fubase A content | 38% | 20% |
Result shows, compared to conventional organic solvent extraction+acid, put forward the alkaloid preparation technology that alkali is heavy, experimental group acid extraction+cationic resin column purifying process of the present invention has reduced the loss of Guan-fubase A in leaching process, and in its extract, the content of Guan-fubase A is significantly higher than control group.
Embodiment
Embodiment 1
2kg Typhoniun Tuber medicinal material, pulverize, with 60L0.5%(w/w) hydrochloric acid diacolation extracts 48 hours, extracting solution is adsorbed in 8L001 * 7 Zeo-karb, take out resin, dry, resin take strong aqua alkalize to pH be 9, resin after alkalization is with 15L chloroform and methyl alcohol (5:1) mixed solvent refluxing extraction 3 times, after extracting solution is concentrated, add oxalic acid to pH be 1, precipitation, filter, precipitation is with water furnishing pasty state, strong aqua alkalize to pH be 8, 50 ℃ dry, with 30ml Virahol, redissolve again, standing crystallization, obtain coarse-grain, coarse-grain is with Virahol-acetone (1:2) recrystallization, filter, dry, obtain Guan-fubase A 5.8g, yield 2.9 ‰, purity 98.6%.
Embodiment 2
1kg Typhoniun Tuber medicinal material, pulverize, gradation is with 10L, 8L, 8L1%(w/w) hydrochloric acid reflux extracts three times, merge, be adsorbed in 5L001 * 7 Zeo-karb, take out resin, dry, resin take strong aqua alkalize to pH be 9, resin after alkalization is with 15L chloroform and ethanol (2:1) mixed solvent refluxing extraction 3 times, after extracting solution is concentrated, add oxalic acid to pH be 2, precipitation, filter, precipitation is with water furnishing pasty state, strong aqua alkalize to pH be 8, 50 ℃ dry, with 100ml dehydrated alcohol, redissolve again, enriching hcl acidifying to pH be 1, standing crystallization, obtain coarse-grain, coarse-grain is with dehydrated alcohol recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 2.6g, yield 2.6 ‰, purity is 98%.
Embodiment 3
5kg Typhoniun Tuber medicinal material, pulverize, with 200L0.1% sulfuric acid diacolation, extract 24 hours, extracting solution is adsorbed in 25LAmberlite IR-20 Zeo-karb, take out resin, dry, resin take strong aqua alkalize to pH be 10, resin after alkalization is with 100L ethyl acetate and methyl alcohol (1:1) mixed solvent refluxing extraction 3 times, after extracting solution is concentrated, add tartrate to pH be 3, precipitation, filter, with water furnishing pasty state, strong aqua alkalize to pH be 10, 50 ℃ dry, with Virahol, redissolve, it is 3 that concentrated hydrochloric acid is acidified to pH, standing crystallization, coarse-grain is with Virahol recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 11.8g, yield 2.36 ‰, purity is 98.4%.
Embodiment 4
3kg Typhoniun Tuber medicinal material, pulverize, with 120L0.5% hydrochloric acid diacolation, extract, extracting solution is adsorbed in 10LD072 type Zeo-karb, take out resin, dry, resin alkalizes with strong aqua, resin after alkalization is with 40L propyl carbinol and acetone (1:2) mixing solutions refluxing extraction 3 times, after extracting solution is concentrated, add citric acid to pH be 2, precipitation, filter, precipitation is with water furnishing pasty state, strong aqua alkalize to pH be 11, 50 ℃ dry, with methyl alcohol and alcohol mixed solvent, dissolve, enriching hcl acidifying to pH be 5, standing crystallization, coarse-grain is with dehydrated alcohol and ethyl acetate mixed solvent recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 7.6g, yield 2.5 ‰, purity is 98.1%.
Embodiment 5
600g Typhoniun Tuber medicinal material, pulverize, respectively with 4.8L, 4.8L, 6L3% oxalic acid refluxing extraction, extracting solution is adsorbed in 3LD151 type Zeo-karb, take out resin, dry, resin take strong aqua alkalize to pH be 9, air-dry, resin after air-dry is with 15L methyl alcohol, ethyl acetate and ether mixed solvent refluxing extraction 3 times, after extracting solution is concentrated, add oxalic acid acidifying, precipitation, filter, precipitation is with water furnishing pasty state, strong aqua alkalize to pH be 9, 50 ℃ dry, with Virahol, redissolve, enriching hcl acidifying to pH be 2, standing crystallization, coarse-grain is with propyl carbinol recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 1.9g, yield 3.16 ‰, purity is 98.0%.
Embodiment 6
By 10kg Typhoniun Tuber pulverizing medicinal materials, respectively with 80L, 80L, 100L1% hydrochloric acid divides refluxing extraction three times, after cooling, extracting solution is adsorbed in 50L001 * 7 type Zeo-karb, take out resin, dry, resin take strong aqua alkalize to pH be 10, air-dry, resin after air-dry is with 200L ethyl acetate and ethanol (3:7) mixed solvent refluxing extraction, the acidifying of extracting solution tartarize, precipitation, filter, precipitation is with water furnishing pasty state, strong aqua alkalize to pH be 10, 40 ℃ dry, with propyl carbinol, dissolve, enriching hcl acidifying to pH be 3, standing crystallization, coarse-grain is with Virahol and acetone (2:1) mixed solvent recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 25g, yield 2.5 ‰, purity 98.3%.
Embodiment 7
Method by embodiment 1-6 and prior art CN1088827A embodiment 1-3 is prepared Guan-fubase A (or its salt), calculates yield and compares crystallizing cycle, the results are shown in Table 2.
Table 2 different methods Guan-fubase A (or its salt) yield and crystallization time comparison
Result shows, the inventive method, in the situation that guaranteeing Guan-fubase A (or its salt) yield, has shortened crystallizing cycle greatly, and its crystallization time is only 1/10 of prior art.
Claims (10)
1. a preparation method for Guan-fubase A, is characterized in that, the method comprises the steps:
Step 1: get Typhoniun Tuber medicinal material acid extraction, obtain extracting solution A;
Step 2: the extracting solution A that step 1 is obtained carries out purifying by resin cation (R.C.), obtains purified;
Step 3: the purified that step 2 is obtained adds organic acid, precipitation, taking precipitate carries out alkalinisation treatment and obtains Guan-fubase A crude product; And
Step 4: the Guan-fubase A crude product that step 3 obtains carries out recrystallization, obtains.
2. a preparation method for Guan-fubase A salt, is characterized in that, the method comprises the steps:
Step 1: get Typhoniun Tuber medicinal material acid extraction, obtain extracting solution A;
Step 2: the extracting solution A that step 1 is obtained carries out purifying by resin cation (R.C.), obtains purified (alkaloids substance);
Step 3: the purified that step 2 is obtained adds organic acid, precipitation, obtains throw out, and taking precipitate carries out alkalinisation treatment and obtains Guan-fubase A crude product; And
Step 4: the Guan-fubase A crude product that step 3 is obtained redissolves with organic solvent, adding acid solution to regulate pH is 1-6, with organic solvent recrystallization, obtains Guan-fubase A salt.
3. method as claimed in claim 1 or 2, is characterized in that, sour water is selected from any one in the hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, oxalic acid of 0.1-3% described in step 1.
As claim 12 or as described in method, it is characterized in that, extracting method is selected from dipping extraction, diacolation extraction, refluxing extraction, supersound extraction any one described in step 1.
5. method as claimed in claim 1 or 2, is characterized in that, Zeo-karb purifying is described in step 2: step 1 extracting solution A is adsorbed in to Zeo-karb, to be exchangedly resin is taken out after completely, alkalization, with organic solvent extraction, reclaims solvent and obtains purified;
Wherein, described Zeo-karb comprises and take any one strongly-acid that is framework material or weakly acidic cation-exchange resin in vinylbenzene, divinylbenzene, acrylate or methacrylic ester;
Described alkalization is selected from any one in sodium hydroxide solution, potassium hydroxide solution, strong aqua or sodium carbonate solution with solution, alkalizes to pH8-12;
Described extraction is one or more the mixed solvent in chloroform, methyl alcohol, ethanol, propyl alcohol, butanols, ethyl acetate, ritalin, acetone, ether with organic solvent.
6. method as claimed in claim 1 or 2, is characterized in that, organic acid is selected from any one in oxalic acid, tartrate, citric acid described in step 3.
7. method as claimed in claim 6, is characterized in that, being acidified to pH is 1-4.
8. method as claimed in claim 1 or 2, is characterized in that, described in step 3 taking precipitate alkalize to pH be 8-11.
9. method as claimed in claim 1 or 2, is characterized in that, throw out carries out drying or cryodrying after alkalinisation treatment described in step 3; Described cryodrying temperature is not higher than 50 ℃.
10. method as claimed in claim 1 or 2, is characterized in that, the organic solvent of recrystallization is one or more the mixture in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol, chloroform, ethyl acetate and acetone described in step 4.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088827A (en) * | 1993-01-01 | 1994-07-06 | 中国药科大学 | A kind of preparation method of diterpene alkaloid and medicinal usage thereof |
| CN102172361A (en) * | 2008-08-13 | 2011-09-07 | 北京和润创新医药科技发展有限公司 | Method for separating traditional Chinese medicine total alkaloids by ion exchange resin |
| CN102757429A (en) * | 2012-07-12 | 2012-10-31 | 李昌禹 | Process for producing acehytisine hydrochloride by biologically converting aconitum coreanum hair root |
-
2013
- 2013-03-25 CN CN201310097092.5A patent/CN104072496B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1088827A (en) * | 1993-01-01 | 1994-07-06 | 中国药科大学 | A kind of preparation method of diterpene alkaloid and medicinal usage thereof |
| CN102172361A (en) * | 2008-08-13 | 2011-09-07 | 北京和润创新医药科技发展有限公司 | Method for separating traditional Chinese medicine total alkaloids by ion exchange resin |
| CN102757429A (en) * | 2012-07-12 | 2012-10-31 | 李昌禹 | Process for producing acehytisine hydrochloride by biologically converting aconitum coreanum hair root |
Non-Patent Citations (1)
| Title |
|---|
| 徐任生 主编: "《天然产物化学》", 30 September 2004, 科学出版社 * |
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Inventor after: Sun Yaling Inventor after: Zeng Yan Inventor after: Sun Shenguo Inventor after: Zhu Tianquan Inventor after: Cheng Zhiguo Inventor after: Jia Jingquan Inventor before: Dong Xiuhua Inventor before: Sun Yaling Inventor before: Zeng Yan Inventor before: Li Na Inventor before: Sun Shenguo Inventor before: Cheng Zhiguo Inventor before: Jia Jingquan |
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Free format text: CORRECT: INVENTOR; FROM: DONG XIUHUA SUN YALING CENG YAN LI NA SUN SHENGUO CHENG ZHIGUO JIA JINGQUAN TO: SUN YALING CENG YAN SUN SHENGUO ZHU TIANQUAN CHENG ZHIGUO JIA JINGQUAN |
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