CN102093345B - Method for separating out dehydrogenized turkey corn by applying silicagel column chromatography - Google Patents
Method for separating out dehydrogenized turkey corn by applying silicagel column chromatography Download PDFInfo
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- CN102093345B CN102093345B CN 201010598262 CN201010598262A CN102093345B CN 102093345 B CN102093345 B CN 102093345B CN 201010598262 CN201010598262 CN 201010598262 CN 201010598262 A CN201010598262 A CN 201010598262A CN 102093345 B CN102093345 B CN 102093345B
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- chloroform
- dehydrocorydaline
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Abstract
The invention discloses a method for separating out dehydrogenized turkey corn by applying silicagel column chromatography. The method comprises the following steps: (1) adding chloroform in taken 200-300 meshes silicagel, stirring and then pouring the mixture in a chromatography column, and mounting the chromatography column; (2) dissolving ethanol crude extract of rhizome corydalis with a mixed solvent of little chloroform and methyl alcohol at a volume ratio of 50:1, producing sample solution and loading the sample, successively carrying out gradient elution with eluant of chloroform and methyl alcohol at a volume ratio of 50:1, 40:1 and 30:1, wherein the flow speed of the eluant is 1.6-2.5 ml/min, collecting eluent in equi-volume, merging the eluent in which the relative front (Rf) value and retention time are the same as that of dehydrogenized turkey corn standard product and the purify of dehydrogenized turkey corn is larger than 90%, recovering solvent with a rotary evaporator so as to obtain crude dehydrogenized turkey corn; and (3) crystallizing the obtained crude dehydrogenized turkey corn by using methyl alcohol or chloroform after the crude dehydrogenized turkey corn is decolored, so that pure dehydrogenized turkey corn is obtained. The method has the advantages of simple process and high recovery, and the purity of the dehydrogenized turkey corn obtained by separation is high.
Description
(1) technical field
The present invention relates to the applying silicon plastic column chromatography and from the corydalis tuber crude extract, separate the method that obtains the high purity Dehydrocorydaline.
(2) background technology
Corydalis tuber (Corydalis yanhusuo W.T.Wang) is the dry tuber of papaveracease (Popaveraceae) plant Yanhusuo, nature and flavor are hot, bitter, warm, return liver, the spleen channel, main product in Zhejiang, the provinces such as Jiangsu, Anhui, Sichuan, corydalis tuber is one of famous " Zhejiang eight flavors ".Corydalis tuber have invigorate blood circulation, the effect of sharp gas, pain relieving, can be used for the chest side of body, epigastric pain, through closing dysmenorrhoea, postpartum stasis blocking, tumbling and swelling.Modern study shows that corydalis tuber effective constituent mainly is alkaloid, it is reported, alkaloid nearly more than 40 is planted in the corydalis tuber, mainly comprises: the tens of kinds of alkaloids such as tetrahydropalmatine, protopine, Dehydrocorydaline (Dehydrocorydaline).The modern pharmacology experiment has proved that tetrahydropalmatine is main analgesia, calm composition in the contained alkaloid of corydalis tuber; Dehydrocorydaline has the expansion coronary vasodilator; improve coronary flow; improve the Nutritional myocardium blood flow amount; strengthen the effects such as myocardial hypoxia tolerance and Ischemic myocardium, necrosis, be the effective constituent for the treatment of coronary heart diseases and angina pectoris medicine corydalis tuber preparation " Kedaling ".In addition, Dehydrocorydaline has also been obtained preferably curative effect in the treatment Peptic Ulcers.
At present, the separation of bibliographical information Dehydrocorydaline has two kinds: a kind of is the application standard high speed adverse current chromatogram, and this method applied sample amount is little, and the instrument that uses is expensive, is difficult to be used widely; Another kind is the various column chromatographies of integrated use (macroporous adsorbent resin, aluminum oxide column chromatography and gel column chromatographies), this method complex steps, and efficient is low, and through chromatography repeatedly, the dead absorption of sample is larger.
(3) summary of the invention
The method that the purpose of this invention is to provide a kind of separating high-purity Dehydrocorydaline, the method technique is simple, and separation efficiency is high, can be used for suitability for industrialized production.
Technical scheme of the present invention is as follows:
A kind of applying silicon plastic column chromatography separates the method for Dehydrocorydaline, said method comprising the steps of:
(1) gets 200～300 purpose silica gel, add chloroform and stir, place the ultrasonator vibration not fill post to having to pour chromatography column into behind the bubble, obtain silicagel column;
(2) with a small amount of chloroform of the alcohol extracts of corydalis tuber, the methyl alcohol volume ratio is 50: 1 dissolution with solvents of mixing, make need testing solution, get need testing solution as the sample solution loading, make sample solution be adsorbed on the silica gel fully, in the described sample solution in the alcohol extracts of corydalis tuber and the silicagel column mass ratio of silica gel be 1: 30～105, use successively chloroform, the methyl alcohol volume ratio is eluent wash-out 150～250min of 50: 1, chloroform, eluent wash-out 150～250min of 40: 1 of methyl alcohol volume ratio, chloroform, 30: 1 eluent of methyl alcohol volume ratio is eluted to thin-layer chromatography and follows the tracks of and to detect to the elutriant without the Dehydrocorydaline component, the eluent flow velocity is 1.6～2.5ml/min, equal-volume is collected elutriant, the elutriant that collection is obtained detects with thin-layer chromatography and high performance liquid chromatography, merges and Dehydrocorydaline standard substance R
fValue and retention time is identical and Dehydrocorydaline purity greater than 90% elutriant, reclaim solvent with Rotary Evaporators, obtain the Dehydrocorydaline crude product;
(3) behind the Dehydrocorydaline crude product depigmentation that obtains of step (2) with methyl alcohol or chloroform crystallization, obtain the Dehydrocorydaline sterling.
The alcohol extracts of described corydalis tuber makes as follows: get the corydalis tuber pulverizing medicinal materials, with 60～98% alcohol reflux 1～5 time, the extracting solution that merges each time, the suction filtration rear filtrate is evaporated to the medicinal extract shape, be 2～3 with the acid solution adjust pH, left standstill 10～30 hours, and got supernatant liquid filtering and remove precipitation; Filtrate is used chloroform extraction 1～5 time, collects the combined chloroform layer, and rotary evaporation reclaims chloroform, gets the alcohol extracts of corydalis tuber.
Described acid solution is that mass concentration is 1～2% aqueous hydrochloric acid or 1～2% aqueous sulfuric acid.
In the described step (3), the method for Dehydrocorydaline crude product depigmentation is one of following:
(A) the Dehydrocorydaline crude product is used dropper sucking-off pigment with a small amount of anhydrous alcohol solution pigment, and residuum with methyl alcohol or chloroform crystallization, obtains the Dehydrocorydaline sterling again;
(B) the Dehydrocorydaline crude product is dissolved in methyl alcohol, add a small amount of gac, the quality consumption of gac is counted 0.01～0.02g/ml with the gained liquor capacity usually, stir 45～60min, remove by filter gac, get the desolventizing of filtrate rotary evaporation, residuum with methyl alcohol or chloroform crystallization, obtains the Dehydrocorydaline sterling again.
The dress post is to add chloroform to stir in silica gel in the described step (1), places the ultrasonator vibration not fill post to having to pour chromatography column into behind the bubble, and is forced into the silica gel face with the duplex ball and no longer descends.
In the described step (2) loading be until chloroform with after the silica gel face flushes, be adsorbed on the silica gel fully with dropper dropping sample solution to sample.
Alcohol extracts with corydalis tuber in the described step (2) is the dissolution with solvents of mixing at 50: 1 with a small amount of chloroform, methyl alcohol volume ratio, describedly refer on a small quantity just can make the consoluet amount of alcohol extracts of corydalis tuber to get final product, this is that those skilled in the art can understand.
The testing conditions of high performance liquid chromatography is in the described step (2): ODS C
18Column (4.6 * 250mm, 5 μ m); Column temperature: 30 ℃; Moving phase: acetonitrile-0.03mol/L SODIUM PHOSPHATE, MONOBASIC (32: 68, v/v), isocratic elution; Flow velocity: 0.6ml/min; Detect wavelength: 345nm; Sample size: 20 μ l.
The Dehydrocorydaline sterling that obtains can further detect with above-mentioned high performance liquid chromatography testing conditions, further determines that it is Dehydrocorydaline, and purity is greater than 98%.
Beneficial effect of the present invention is: the present invention separates the Dehydrocorydaline purity height that obtains, and technique is simple, and the rate of recovery is high, and taking full advantage of of corydalis tuber medicinal material played an important role.
(4) embodiment
The present invention will be further described with specific embodiment for the below, but protection scope of the present invention is not limited to this.
Embodiment 1
After getting corydalis tuber medicinal material 1500g and pulverizing with 70% alcohol reflux of 22.5L 30 minutes, pressing same method extracts 3 times, merge 3 times extracting solution, the suction filtration rear filtrate is evaporated to the medicinal extract shape, is 3 with 2% hydrochloric acid soln adjust pH, leaves standstill 15h, suction filtration, filtrate is reclaimed chloroform with 4 * 400mL chloroform extraction, combined chloroform layer with Rotary Evaporators, gets corydalis tuber crude extract 10.4g.
Take by weighing 200-300 order silica gel 25g, add the 300mL chloroform, stir, place the ultrasonator vibration not fill post to having to pour chromatography column into behind the bubble, obtain silicagel column.
Take by weighing corydalis tuber crude extract 239mg (sample and silica gel ratio are 1: 105), with 4mL eluent (chloroform-methanol=50: 1 (v/v)) dissolving, get sample solution.
Whole sample solutions are added drop-wise to Silica Surface and make it be adsorbed in silica gel fully with dropper.
Be 50: 1 40: 1 eluent wash-out 250min of eluent wash-out 250min, chloroform, methyl alcohol volume ratio successively with chloroform, methyl alcohol volume ratio, chloroform, 30: 1 eluent of methyl alcohol volume ratio are eluted to thin-layer chromatography and follow the tracks of and to detect to the elutriant without the Dehydrocorydaline component, the eluent flow velocity is 2.5ml/min, collect elutriant with Erlenmeyer flask, every 50ml collects one bottle, the elutriant that collection is obtained detects with thin-layer chromatography and high performance liquid chromatography, merges and Dehydrocorydaline standard substance R
fValue and retention time is identical and Dehydrocorydaline purity greater than 90% elutriant, reclaim solvent with Rotary Evaporators, obtain the Dehydrocorydaline crude product.
Dehydrocorydaline crude product 3mL anhydrous alcohol solution pigment, with dropper with its sucking-off, remaining composition 5mL methanol crystallization, obtain yellow crystals 26mg, the crystal that obtains is carried out high performance liquid chromatography to be detected, further determine that it is Dehydrocorydaline, purity is 99.6%, and the rate of recovery is 84.9% (in the corydalis tuber crude extract).
The testing conditions of high performance liquid chromatography is: ODS C
18Column (4.6 * 250mm, 5 μ m); Column temperature: 30 ℃; Moving phase: acetonitrile-0.03mol/L SODIUM PHOSPHATE, MONOBASIC (32: 68, v/v), isocratic elution; Flow velocity: 0.6ml/min; Detect wavelength: 345nm; Sample size: 20 μ l.
Embodiment 2
Take by weighing 200-300 order silica gel 20g, add the 250mL chloroform, stir, place the ultrasonator vibration not fill post to having to pour chromatography column into behind the bubble, obtain silicagel column.
Take by weighing embodiment 1 and extract the corydalis tuber crude extract 368mg (sample and silica gel ratio are 1: 54) that obtains, with 5mL eluent (chloroform-methanol=50: 1 (v/v)) dissolving, get sample solution.
Whole sample solutions are added drop-wise to Silica Surface and make it be adsorbed in silica gel fully with dropper.
Be 50: 1 40: 1 eluent wash-out 200min of eluent wash-out 150min, chloroform, methyl alcohol volume ratio successively with chloroform, methyl alcohol volume ratio, chloroform, 30: 1 eluent of methyl alcohol volume ratio are eluted to thin-layer chromatography and follow the tracks of and to detect to the elutriant without the Dehydrocorydaline component, the eluent flow velocity is 2.0ml/min, collect elutriant with Erlenmeyer flask, every 50ml collects one bottle, the elutriant that collection is obtained detects with thin-layer chromatography and high performance liquid chromatography, merges and Dehydrocorydaline standard substance R
fValue and retention time is identical and Dehydrocorydaline purity greater than 90% elutriant, reclaim solvent with Rotary Evaporators, obtain the Dehydrocorydaline crude product.
Dehydrocorydaline crude product 40mL dissolve with methanol, add the 0.4g gac, stir 45min, remove by filter gac, get the desolventizing of filtrate rotary evaporation, residuum is used the 6mL methanol crystallization again, obtain yellow crystals 37mg, determine that it is Dehydrocorydaline, purity 99.6%, the rate of recovery 78.4% (in the corydalis tuber crude extract) through the high performance liquid phase detection.
The testing conditions of high performance liquid chromatography is: ODS C
I8Column (4.6 * 250mm, 5 μ m); Column temperature: 30 ℃; Moving phase: acetonitrile-0.03mol/L SODIUM PHOSPHATE, MONOBASIC (32: 68, v/v), isocratic elution; Flow velocity: 0.6ml/min; Detect wavelength: 345nm; Sample size: 20 μ l.
Embodiment 3
Take by weighing 200-300 order silica gel 9g, add the 200mL chloroform, stir, place the ultrasonator vibration not fill post to having to pour chromatography column into behind the bubble, obtain silicagel column.
Take by weighing embodiment 1 and extract the corydalis tuber crude extract 296mg (sample and silica gel ratio are 1: 30) that obtains, with 4mL eluent (chloroform-methanol=50: 1 (v/v)) dissolving, get sample solution.
Whole sample solutions are added drop-wise to Silica Surface and make it be adsorbed in silica gel fully with dropper.
Use successively chloroform, the methyl alcohol volume ratio is 50: 1 eluent wash-out 150min, chloroform, 40: 1 eluent wash-out 150min of methyl alcohol volume ratio, chloroform, 30: 1 eluent of methyl alcohol volume ratio is eluted to thin-layer chromatography and follows the tracks of and to detect to the elutriant without the Dehydrocorydaline component, the eluent flow velocity is 1.6ml/min, collect elutriant with Erlenmeyer flask, every 50ml collects one bottle, the elutriant that collection is obtained detects with thin-layer chromatography and high performance liquid chromatography, merge with Dehydrocorydaline standard substance Rf value and retention time is identical and Dehydrocorydaline purity greater than 90% elutriant, reclaim solvent with Rotary Evaporators, obtain the Dehydrocorydaline crude product.
Dehydrocorydaline crude product 55mL dissolve with methanol, add the 1.1g gac, stir 60min, remove by filter gac, get the desolventizing of filtrate rotary evaporation, residuum is used the crystallization of 5mL chloroform again, obtain yellow crystals 30mg, be defined as Dehydrocorydaline through the high performance liquid phase detection, purity 99.4%, the rate of recovery are 78.9% (in the corydalis tuber crude extract).
The testing conditions of high performance liquid chromatography is: ODS C
18Column (4.6 * 250mm, 5 μ m); Column temperature: 30 ℃; Moving phase: acetonitrile-0.03mol/L SODIUM PHOSPHATE, MONOBASIC (32: 68, v/v), isocratic elution; Flow velocity: 0.6ml/min; Detect wavelength: 345nm; Sample size: 20 μ l.
Claims (4)
1. an applying silicon plastic column chromatography separates the method for Dehydrocorydaline, it is characterized in that said method comprising the steps of:
(1) gets 200 ~ 300 purpose silica gel, add chloroform and stir, place the ultrasonator vibration not fill post to having to pour chromatography column into behind the bubble, obtain silicagel column;
(2) with a small amount of chloroform of the alcohol extracts of corydalis tuber, the methyl alcohol volume ratio is the dissolution with solvents that 50:1 mixes, make need testing solution, get need testing solution as the sample solution loading, make sample solution be adsorbed on the silica gel fully, in the described sample solution in the alcohol extracts of corydalis tuber and the silicagel column mass ratio of silica gel be 1:30～105, use successively chloroform, the methyl alcohol volume ratio is eluent wash-out 150 ~ 250min of 50:1, chloroform, eluent wash-out 150 ~ 250min of methyl alcohol volume ratio 40:1, chloroform, the eluent of methyl alcohol volume ratio 30:1 is eluted to thin-layer chromatography and follows the tracks of and to detect to the elutriant without the Dehydrocorydaline component, the eluent flow velocity is 1.6 ~ 2.5ml/min, equal-volume is collected elutriant, the elutriant that collection is obtained detects with thin-layer chromatography and high performance liquid chromatography, merges and Dehydrocorydaline standard substance R
fValue and retention time is identical and Dehydrocorydaline purity greater than 90% elutriant, reclaim solvent with Rotary Evaporators, obtain the Dehydrocorydaline crude product;
The alcohol extracts of described corydalis tuber makes as follows: get the corydalis tuber pulverizing medicinal materials, with 60～98% alcohol reflux 1～5 time, the extracting solution that merges each time, the suction filtration rear filtrate is evaporated to the medicinal extract shape, be 2～3 with the acid solution adjust pH, left standstill 10 ~ 30 hours, and got supernatant liquid filtering and remove precipitation; Filtrate is used chloroform extraction 1 ~ 5 time, collects the combined chloroform layer, and rotary evaporation reclaims chloroform, gets the alcohol extracts of corydalis tuber;
(3) behind the Dehydrocorydaline crude product depigmentation that obtains of step (2) with methyl alcohol or chloroform crystallization, obtain the Dehydrocorydaline sterling.
2. the method for claim 1 is characterized in that described acid solution is that mass concentration is 1～2% aqueous hydrochloric acid or 1～2% aqueous sulfuric acid.
3. the method for claim 1 is characterized in that in the described step (3), is one of following with the method for methyl alcohol or chloroform crystallization behind the Dehydrocorydaline crude product depigmentation:
(A) the Dehydrocorydaline crude product is used dropper sucking-off pigment with a small amount of anhydrous alcohol solution pigment, and residuum with methyl alcohol or chloroform crystallization, obtains the Dehydrocorydaline sterling again;
(B) the Dehydrocorydaline crude product is dissolved in methyl alcohol, adds a small amount of gac, stirs 45～60 min, removes by filter gac, gets the desolventizing of filtrate rotary evaporation, and residuum with methyl alcohol or chloroform crystallization, obtains the Dehydrocorydaline sterling again.
4. the method for claim 1 is characterized in that the testing conditions of high performance liquid chromatography in the described step (2) is: ODS C
18Column 4.6 * 250 mm, 5 μ m; Column temperature: 30 ℃; Moving phase: acetonitrile-0.03mol/L SODIUM PHOSPHATE, MONOBASIC, volume ratio are 32:68, isocratic elution; Flow velocity: 0.6 ml/min; Detect wavelength: 345nm; Sample size: 20 μ l.
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| CN103616344B (en) * | 2013-12-12 | 2016-03-16 | 山东金诃药物研究开发有限公司 | A kind of detection method of Tibetan medicine material Corydalis impatiens (Pall.) Fisch |
| CN109503571A (en) * | 2018-12-06 | 2019-03-22 | 金华职业技术学院 | A kind of method of dehydrocorydaline in D101 macroporous resin purification rhizoma corydalis |
| CN114088829B (en) * | 2021-11-04 | 2023-06-23 | 天津中医药大学 | Method for detecting dehydrocorydaline and metabolic products thereof and application of method |
| CN116602966A (en) * | 2023-05-11 | 2023-08-18 | 华宝民康(广东)医药集团有限公司 | Application of 13-methyl-palmatine in preparation of medicines for resisting myocardial ischemia injury and heart fibrosis |
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| CN1634295A (en) * | 2004-09-27 | 2005-07-06 | 方芳 | Preparation method for climbing nightshade extract |
| CN101480394A (en) * | 2008-01-09 | 2009-07-15 | 上海安普生物科技有限公司 | Anti-tumor pharmaceutical composition |
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