CN104072496B - The preparation method of a kind of Guan-fubase A and salt thereof - Google Patents
The preparation method of a kind of Guan-fubase A and salt thereof Download PDFInfo
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- CN104072496B CN104072496B CN201310097092.5A CN201310097092A CN104072496B CN 104072496 B CN104072496 B CN 104072496B CN 201310097092 A CN201310097092 A CN 201310097092A CN 104072496 B CN104072496 B CN 104072496B
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- C07—ORGANIC CHEMISTRY
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- 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 present invention provides the preparation method of a kind of Guan-fubase A and salt thereof. The method adopts acid extraction to purify the technique combined with cation-adsorption resin, impurity is removed again with organic acid precipitation, recrystallization obtains Guan-fubase A and salt thereof, and the method comprises the steps: step 1 specifically: gets Typhoniun Tuber medicinal material acid extraction, obtains extracting solution A; Step 2: extracting solution A carries out purifying by resin cation (R.C.), obtains purified step 3: purified step 2 obtained adds organic acid, precipitation, 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 obtains carries out recrystallization. The method improves the content of Guan-fubase A in product fast, greatly shortens crystallizing cycle.
Description
Technical field
The present invention provides the method for a kind of extraction and isolation Guan-fubase A and salt thereof from herbal medicine, is specifically related to the method for a kind of extraction and isolation Guan-fubase A and salt thereof from Radix Aconiti Coreani.
Background technology
Typhoniun Tuber is the block root of Chinese medicine Ranunculaceae Radix Aconiti Coreani Aconitumcoreanum (L �� vl.) Rapaics, is one of conventional Chinese medicine, and Typhoniun Tuber is used for arthralgia due to cold-dampnes by tcm clinical practice for many years, migraine, and waist knee joint crymodynia etc., achieve good results. Modern pharmacological research shows that in Typhoniun Tuber, main active ingredient is C20Diterpenes alkaloid compound, mainly comprises and closes attached element in heptan (GuanfubaseG, GFG), and Guan-fubase A (GuanfubaseA, GFA), closes attached element in the ninth of the ten Heavenly Stems (GuanfubaseI, GFI) etc.
Clinical front pharmacological research shows: Guan-fu base A hydrochloride can resist ventricular tachycardia and the ventricular fibrillation that high calcium, ligation coronary artery and napelline bring out, and the auricular flutter that anti-acetylcholine can be brought out and atrial fibrillation; The V to cardiac muscle fast response action potential can be reduced by concentration dependentmax. It is main polyion channeling that the full cell method of patch clamp proves that this Drug inhibition reacts stream in the Na+ of myocardial cell soon, is the natural product of a good anti-heart disorder. A large amount of clinical data shows, Guan-fu base A hydrochloride is the active drug of tachycardia and ventricular arythmia on treatment paroxysmal room, certainly, untoward reaction is few and slight, is the safe and effective wide spectrum anti-heart disorder Western medicine one original new drug of class of the brand new type of Late Cambrian for curative effect.
The method of prior art many employings multistep extraction prepares Guan-fu base A hydrochloride, and Chinese patent CN1088827A discloses the preparation technology of Guan-fubase A, and this technique ethanol extraction yield is low, and defatting step have employed a large amount of organic solvent, and environmental pollution is serious; Extraction step emulsification is serious, and extraction efficiency is low; Wherein using the method for column chromatography, Guan-fubase A loss is big, equipment requirements height, complex operation step, and Guan-fubase A yield is low; Crystallisation step carries out in the more situation of impurity, crystallization difficulty, crystallizing cycle very long (several weeks), and yield is lower.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of Guan-fubase A.
It is an object of the invention to provide the preparation method of a kind of Guan-fubase A salt.
It is an object of the invention 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, obtains extracting solution A;
Step 2: extracting solution A, by resin cation (R.C.) purifying, obtains purified (alkaloids substance);
Step 3: purified step 2 obtained adds organic acid, precipitation, obtains throw out, obtains Guan-fubase A crude product after being alkalized by throw out;
Step 4: step 3 gained Guan-fubase A crude product carries out recrystallization.
Further, acid water described in step 1 be selected from the hydrochloric acid of 0.1-3%, sulfuric acid, nitric acid, phosphoric acid, oxalic acid any one; The hydrochloric acid of preferred 0.1-3%. Acid water consumption is medicinal material: acid water (kg/L)=1:20-40.
Further, extracting method described in step 1 be selected from Soakage extraction, seepage pressure effects, refluxing extraction, supersound extraction any one; Preferred seepage pressure effects or refluxing extraction.
Further, described in step 2, Zeo-karb purifying is: step 1 extracting solution A is adsorbed in Zeo-karb, to be exchanged completely after resin is taken out, alkalization, with organic solvent extraction, recycling design obtains purified (alkaloids substance); Wherein, described Zeo-karb comprises in vinylbenzene, divinylbenzene, acrylate or methacrylic ester any one as the strongly-acid of framework material or weakly acidic cation-exchange resin; It it is preferably the storng-acid cation exchange resin of framework material taking vinylbenzene; Described alkalization solution be selected from sodium hydroxide solution, potassium hydroxide solution, strong aqua or sodium carbonate solution any one, alkalization to the preferred pH10-12 of pH8-12(); Described extraction organic solvent is the mixed solvent of one or more in chloroform, methyl alcohol, ethanol, propyl alcohol, butanols, ethyl acetate, ritalin, acetone, ether; It is 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, organic acid described in step 3 be selected from oxalic acid, tartrate, citric acid any one; Being acidified to pH is the preferred pH1-3 of 1-4().
Further, taking precipitate described in step 3 carry out alkalizing to pH be the preferred pH9-11 of 8-11().
Further, throw out described in step 3 carries out drying or cryodrying after carrying out alkalinisation treatment; Further, described cryodrying temperature is not higher than 50 DEG C.
Further, the organic solvent of recrystallization described in step 4 is the mixture of one or more in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol, chloroform, ethyl acetate and acetone.
Further, the preparation method of a kind of Guan-fubase A, the method comprises:
Step 1: get Typhoniun Tuber medicinal material, pulverizes, and oozes with acid water and filters or refluxing extraction, obtains extracting solution A;
Step 2: extracting solution A step 1 obtained is adsorbed in Zeo-karb, to be exchanged completely after resin is taken out, dry, alkalize to pH as 8-12 taking strong aqua, with organic solvent refluxing extraction, recycling design obtains purified (alkaloids substance);
Step 3: it is 1-4 that purified step 2 obtained adds organic acid to pH, precipitation, filters, and taking precipitate adjusts into pasty state with water, and strong aqua alkalization is 8-12 to pH, dry, obtains Guan-fubase A crude product;
Step 4: Guan-fubase A crude product step 3 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: purified step 2 obtained adds organic acid, precipitation, obtains throw out, and taking precipitate carries out alkalinisation treatment and obtains Guan-fubase A crude product;
Step 4: Guan-fubase A crude product step 3 obtained redissolves with organic solvent, adds acid solution and regulates pH to be 1-6, leave standstill analysis brilliant, then with organic solvent recrystallization, obtain Guan-fubase A salt.
Further, acid water described in step 1 be selected from the hydrochloric acid of 0.1-3%, sulfuric acid, nitric acid, phosphoric acid, oxalic acid any one; The hydrochloric acid of preferred 0.1-3%. Acid water consumption is medicinal material: acid water (Kg/L)=1:20-40.
Further, extracting method described in step 1 be selected from Soakage extraction, seepage pressure effects, refluxing extraction, supersound extraction any one; Preferred seepage pressure effects or refluxing extraction.
Further, described in step 2, Zeo-karb purifying is: step 1 extracting solution A is adsorbed in Zeo-karb, to be exchanged completely after resin is taken out, alkalization, with organic solvent extraction, recycling design obtains purified (alkaloids substance); Wherein, described Zeo-karb comprises in vinylbenzene, divinylbenzene, acrylate or methacrylic ester any one as the strongly-acid of framework material or weakly acidic cation-exchange resin; It it is preferably the storng-acid cation exchange resin of framework material taking vinylbenzene; Described alkalization solution be selected from sodium hydroxide solution, potassium hydroxide solution, strong aqua or sodium carbonate solution any one, alkalization to the preferred pH10-12 of pH8-12(); Described extraction organic solvent is the mixed solvent of one or more in chloroform, methyl alcohol, ethanol, propyl alcohol, butanols, ethyl acetate, ritalin, acetone, ether; It is 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, organic acid described in step 3 be selected from oxalic acid, tartrate, citric acid any one; Being acidified to pH is the preferred pH1-3 of 1-4().
Further, taking precipitate described in step 3 carry out alkalizing to pH be the preferred pH9-11 of 8-11().
Further, throw out described in step 3 carries out drying or cryodrying after carrying out alkalinisation treatment; Further, described cryodrying temperature is not higher than 50 DEG C.
Further, the organic solvent of recrystallization described in step 4 is the mixture of one or more in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol, chloroform, ethyl acetate and acetone.
Further, the preparation method of a kind of Guan-fubase A hydrochloride, the method comprises:
Step 1: get Typhoniun Tuber medicinal material, pulverizes, and oozes with acid water and filters or refluxing extraction, obtains extracting solution A;
Step 2: extracting solution A step 1 obtained is adsorbed in Zeo-karb, to be exchanged completely after resin is taken out, dry, alkalize to pH as 8-12 taking strong aqua, with organic solvent refluxing extraction, recycling design obtains purified (alkaloids substance);
Step 3: it is the preferred pH1-3 of 1-4(that purified step 2 obtained adds organic acid to pH), precipitation, filters, and taking precipitate adjusts into pasty state with water, and strong aqua alkalization is 8-11 to pH, dry, obtains Guan-fubase A crude product;
Step 4: Guan-fubase A crude product step 3 obtained redissolves with organic solvent, enriching hcl acidifying is 1-6 to pH, leaves standstill analysis brilliant, then carries out recrystallization with organic solvent, filters, dry, obtains Guan-fubase A hydrochloride.
In addition, present invention also offers one and prepare 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, the technique adopting acid extraction to combine with the purification of cation-adsorption resin extracts Typhoniun Tuber total alkaloids, organic solvent extraction compared to existing technology, not only saves cost, reduces environmental pollution, and decrease the loss of target component Guan-fubase A, it is to increase the extraction yield of Guan-fubase A.
2, avoiding extracting solution concentrated rear directly by the problem that emulsification during organic solvent extraction is serious, equipment requirements is not high, and operability is very strong.
3, directly add the purifying method of Acid precipitation after adopting organic solvent extraction, improve the content of Guan-fubase A in product fast, greatly shorten crystallizing cycle. Compared with prior art, when ensureing Guan-fubase A purity (all reaching more than 98%) and yield (most high yield pulp1 reach 3.16 ��), its crystallizing cycle is only the 1/10 of prior art to the inventive method.
Effect experimental examples
Experimental example 1 Different Extraction Method is on the impact of Guan-fubase A extraction yield
1 sample preparation
Experimental group: get 1kg Typhoniun Tuber medicinal material, broken, 200L0.1% sulfuric acid seepage pressure effects, extracting solution is adsorbed in 25LAmberliteIR-20 Zeo-karb, taking out resin, dry, resin alkalizes to pH as 10 taking strong aqua, resin after alkalization extracts with 100L ethyl acetate and methanol mixed solvent refluxing, and recycling design obtains total alkaloids.
Control group: get 1kg Typhoniun Tuber medicinal material, pulverizes, ethanol percolate extraction, reclaim ethanol, obtain medicinal extract, add 1% dissolving with hydrochloric acid, acid liquid adjusts pH3, leaves standstill acid liquid analysis glue, precipitates in filtering acid liquid, with petroleum ether degreasing, divide and remove petroleum ether layer, alkalize acid liquid to pH5 with dense ammonia, again with chloroform extraction, collecting 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 the solution of every 1ml containing 0.50mg, shake even, to obtain final product.
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 dissolving and be diluted to scale, shake even, filter, get continuous filtrate, to obtain final product.
2.3 chromatographic conditions:
It is weighting agent with octadecylsilane chemically bonded silica; With the sodium heptanesulfonate aqueous solution (containing 0.2% triethylamine, and taking phosphoric acid adjust pH to the 3.0)-acetonitrile (75:25) of 2ml/ml as moving phase; Determined wavelength is 205nm.
3 experimental results
Employing marker method carries out, and measurement result is in table 1.
Table 1 Different Extraction Method Guan-fubase A comparision contents
| Experimental group | Control group | |
| Guan-fubase A content | 38% | 20% |
Result shows, the heavy alkaloid preparation technology of alkali is put forward compared to conventional organic solvent extraction+acid, experimental group acid extraction+cationic resin column purifying process of the present invention decreases 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 seepage pressure effects 48 hours, extracting solution is adsorbed in 8L001 �� 7 Zeo-karb, take out resin, dry, resin alkalizes to pH as 9 taking strong aqua, resin after alkalization is with 15L chloroform and methyl alcohol (5:1) mixed solvent refluxing extraction 3 times, adding oxalic acid to pH after extracting solution is concentrated is 1, precipitation, filter, precipitation adjusts into pasty state with water, strong aqua alkalization is 8 to pH, 50 DEG C of dryings, redissolve with 30ml Virahol again, leave standstill analysis brilliant, obtain coarse-grain, coarse-grain is with Virahol-acetone (1:2) recrystallization, filter, dry, obtain Guan-fubase A 5.8g, receipts rate 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, it is adsorbed in 5L001 �� 7 Zeo-karb, take out resin, dry, resin alkalizes to pH as 9 taking strong aqua, resin after alkalization is with 15L chloroform and ethanol (2:1) mixed solvent refluxing extraction 3 times, adding oxalic acid to pH after extracting solution is concentrated is 2, precipitation, filter, precipitation adjusts into pasty state with water, strong aqua alkalization is 8 to pH, 50 DEG C of dryings, redissolve with 100ml dehydrated alcohol again, enriching hcl acidifying is 1 to pH, leave standstill analysis brilliant, obtain coarse-grain, coarse-grain is with dehydrated alcohol recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 2.6g, receipts rate 2.6 ��, purity is 98%.
Embodiment 3
5kg Typhoniun Tuber medicinal material, pulverize, with 200L0.1% sulfuric acid seepage pressure effects 24 hours, extracting solution is adsorbed in 25LAmberliteIR-20 Zeo-karb, take out resin, dry, resin alkalizes to pH as 10 taking strong aqua, resin after alkalization is with 100L ethyl acetate and methyl alcohol (1:1) mixed solvent refluxing extraction 3 times, adding tartrate to pH after extracting solution is concentrated is 3, precipitation, filter, pasty state is adjusted into water, strong aqua alkalization is 10 to pH, 50 DEG C of dryings, redissolve with Virahol, it is 3 that concentrated hydrochloric acid is acidified to pH, leave standstill analysis brilliant, coarse-grain is with recrystallisation from isopropanol, filter, dry, obtain Guan-fubase A hydrochloride 11.8g, receipts rate 2.36 ��, purity is 98.4%.
Embodiment 4
3kg Typhoniun Tuber medicinal material, pulverize, with 120L0.5% hydrochloric acid seepage pressure effects, 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, adding citric acid to pH after extracting solution is concentrated is 2, precipitation, filter, precipitation adjusts into pasty state with water, strong aqua alkalization is 11 to pH, 50 DEG C of dryings, dissolve with methyl alcohol and alcohol mixed solvent, enriching hcl acidifying is 5 to pH, leave standstill analysis brilliant, coarse-grain is with dehydrated alcohol and ethyl acetate mixed solvent recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 7.6g, receipts rate 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 alkalizes to pH as 9 taking strong aqua, air-dry, resin after air-dry is with 15L methyl alcohol, ethyl acetate and ether mixed solvent refluxing extraction 3 times, oxalic acid acidifying is added after extracting solution is concentrated, precipitation, filter, precipitation adjusts into pasty state with water, strong aqua alkalization is 9 to pH, 50 DEG C of dryings, redissolve with Virahol, enriching hcl acidifying is 2 to pH, leave standstill analysis brilliant, coarse-grain is with propyl carbinol recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 1.9g, receipts rate 3.16 ��, purity is 98.0%.
Embodiment 6
By 10kg Typhoniun Tuber pulverizing medicinal materials, respectively with 80L, 80L, 100L1% hydrochloric acid divides three refluxing extraction, extracting solution is adsorbed in 50L001 �� 7 type Zeo-karb after cooling, take out resin, dry, resin alkalizes to pH as 10 taking strong aqua, air-dry, resin after air-dry is with 200L ethyl acetate and ethanol (3:7) mixed solvent refluxing extraction, extracting solution adds tartrate acidifying, precipitation, filter, precipitation adjusts into pasty state with water, strong aqua alkalization is 10 to pH, 40 DEG C of dryings, with n-Butanol soluble, enriching hcl acidifying is 3 to pH, leave standstill analysis brilliant, coarse-grain is with Virahol and acetone (2:1) mixed solvent recrystallization, filter, dry, obtain Guan-fubase A hydrochloride 25g, receipts rate 2.5 ��, purity 98.3%.
Embodiment 7
Prepare Guan-fubase A (or its salt) by the method for embodiment 1-6 and prior art CN1088827A embodiment 1-3, calculate yield and compare crystallizing cycle, the results are shown in Table 2.
Table 2 different methods Guan-fubase A (or its salt) yield and crystallization time compare
Result shows, the inventive method, when ensureing Guan-fubase A (or its salt) yield, substantially reduces crystallizing cycle, and its crystallization time is only the 1/10 of prior art.
Claims (10)
1. the preparation method of a Guan-fubase A, it is characterised in that, the method comprises the steps:
Step 1: get Typhoniun Tuber medicinal material acid extraction, obtain extracting solution A;
Step 2: extracting solution A step 1 obtained carries out purifying by resin cation (R.C.), obtains purified;
Step 3: purified step 2 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, to obtain final product;
Wherein, described in step 2, Zeo-karb purifying is: step 1 extracting solution A is adsorbed in Zeo-karb, to be exchanged completely after resin is taken out, alkalization, with organic solvent extraction, recycling design obtains purified.
2. the preparation method of a Guan-fubase A salt, it is characterised in that, the method comprises the steps:
Step 1: get Typhoniun Tuber medicinal material acid extraction, obtain extracting solution A;
Step 2: extracting solution A step 1 obtained carries out purifying by resin cation (R.C.), obtains purified;
Step 3: purified step 2 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: Guan-fubase A crude product step 3 obtained redissolves with organic solvent, adds acid solution and regulates pH to be 1-6, with organic solvent recrystallization, obtain Guan-fubase A salt;
Wherein, described in step 2, Zeo-karb purifying is: step 1 extracting solution A is adsorbed in Zeo-karb, to be exchanged completely after resin is taken out, alkalization, with organic solvent extraction, recycling design obtains purified.
3. method as claimed in claim 1 or 2, it is characterised in that, acid water described in step 1 be selected from the hydrochloric acid of 0.1-3%, sulfuric acid, nitric acid, phosphoric acid, oxalic acid any one.
4. method as claimed in claim 1 or 2, it is characterised in that, extracting method described in step 1 be selected from Soakage extraction, seepage pressure effects, refluxing extraction, supersound extraction any one.
5. method as claimed in claim 1 or 2, it is characterised in that, described Zeo-karb comprises in vinylbenzene, divinylbenzene, acrylate or methacrylic ester any one as the strongly-acid of framework material or weakly acidic cation-exchange resin;
Described alkalization solution be selected from sodium hydroxide solution, potassium hydroxide solution, strong aqua or sodium carbonate solution any one, alkalization to pH8-12;
Described extraction organic solvent is the mixed solvent of one or more in chloroform, methyl alcohol, ethanol, propyl alcohol, butanols, ethyl acetate, ritalin, acetone, ether.
6. method as claimed in claim 1 or 2, it is characterised in that, organic acid described in step 3 be selected from oxalic acid, tartrate, citric acid any one.
7. method as claimed in claim 6, it is characterised in that, being acidified to pH is 1-4.
8. method as claimed in claim 1 or 2, it is characterised in that, taking precipitate described in step 3 carry out alkalizing to pH be 8-11.
9. method as claimed in claim 1 or 2, it is characterised in that, throw out described in step 3 carries out drying or cryodrying after carrying out alkalinisation treatment; Described cryodrying temperature is not higher than 50 DEG C.
10. method as claimed in claim 1 or 2, it is characterised in that, the organic solvent of recrystallization described in step 4 is the mixture of one or more in methyl alcohol, ethanol, propyl alcohol, Virahol, propyl carbinol, chloroform, ethyl acetate and acetone.
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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 |
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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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