CN102649782A - Method for extracting griffonilide and thalictricoside from radix semiaquilegiae - Google Patents
Method for extracting griffonilide and thalictricoside from radix semiaquilegiae Download PDFInfo
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- CN102649782A CN102649782A CN2011100453633A CN201110045363A CN102649782A CN 102649782 A CN102649782 A CN 102649782A CN 2011100453633 A CN2011100453633 A CN 2011100453633A CN 201110045363 A CN201110045363 A CN 201110045363A CN 102649782 A CN102649782 A CN 102649782A
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Abstract
The invention relates to a method for extracting griffonilide and thalictricoside from radix semiaquilegiae, which mainly comprises the following steps of: solvent extraction, diatomite decolorization, film separation, column chromatography implementation, re-crystallization and the like, and meanwhile, the griffonilide and the thalictricoside are obtained. The method has the technical effects that firstly, by utilizing the nature that both the griffonilide and the thalictricoside are easily dissolved in methanol, the methanol is adopted for extraction to obtain a total extract; secondly, the extract is separated and concentrated through a biological film to filter a polysaccharide composition, thereby reducing the subsequent operation pressure; and thirdly, by utilizing the polarity difference of the griffonilide and the thalictricoside, adsorption and elution are carried out through macro-porous resin to effectively separate the griffonilide from the thalictricoside. The method has the advantages of simple operation, low cost and high purity of an obtained monomer, thereby laying a material foundation for the pharmological study of two effective components and the quality control of the radix semiaquilegiae and a preparation containing the radix semiaquilegiae.
Description
Technical field:
The invention belongs to the extracted form natural plant field, be specifically related to a kind of method of from Root of Muskroot-like Semiaquilegia, extracting lattice row wind lactone and Dong Fangtangsong leather glycosides.
Background technology:
The dried root of semiaquilegia adoxoides subsystem cohosh semiaquilegia adoxoides Semiaquilegia adoxoides (DC.) Makino, the beginning is stated from Qing Dynasty's ZHAO Xue-Min supplementary Amplifications of the Compendium of Materia Medica, is commonly called as mouse dung in thousand, also claims RADIX SEMIAQUILEGIAE.The Root of Muskroot-like Semiaquilegia aboundresources, it is very wide to distribute, and is found in provinces and regions such as Henan, Jiangsu, Anhui, Zhejiang, Jiangxi, Fujian, Hubei, and main product is in Shaoyang, Hunan, Changsha, enshi, Xuanen, and Jiangsu shakes ground such as pool.Record in " one one of Chinese pharmacopoeia version in 2010 has clearing heat and detoxicatingly, and the effect of dispersing swelling and dissipating binds is used to treat the swollen furunculosis of carbuncle, acute mastitis, scrofula, snake bite and insect sting.Modern pharmacology experiment shows, Root of Muskroot-like Semiaquilegia has restraining effect to streptococcus aureus etc.; Clinically with Root of Muskroot-like Semiaquilegia or its compound treatment acute soft tissue injury and tuberculosis of bone and joint, acute mastitis, hysteromyoma, primary hepatocarcinoma, cancer of the stomach etc.Root of Muskroot-like Semiaquilegia mainly contains vegeto-alkali, lactone, tonka bean camphor, phenolic acid and phenolic glycoside compounds.Wherein lattice row wind lactone and east grass of meadow rue glycosides are relatively more rare in general plant, but the amount in Root of Muskroot-like Semiaquilegia is higher.
Lattice row wind lactone (Griffonilide), molecular formula: C
8H
8O
4, molecular weight: 168.04, for colourless needle (methyl alcohol), be soluble in methyl alcohol, be slightly soluble in water, acetone, be insoluble in chloroform, pharmacological research shows that lattice row wind lactone has significant anti-inflammatory activity, its to the inhibiting rate of inflammation up to 64%.East grass of meadow rue glycosides (thalictricoside) is nitrophenol glycoside composition, molecular formula: C
19H
27NO
12, molecular weight: 461.42, be colourless needle (methyl alcohol).
Lattice row wind lactone east grass of meadow rue glycosides
The ox cutting edge of a knife or a sword adopts 5 times of 95% alcohol heating reflux to extract 3 times, each 3h, extracting solution concentrate medicinal extract; Suspend in water; Use vinyl acetic monomer and n-butanol extraction respectively, ethyl acetate extraction part solvent evaporated, last silicagel column chloroform-methanol wash-out; Chloroform-methanol (100: 8) partially concd crystallization, recrystallizing methanol obtain lattice row wind lactone; N-butanol extraction position water bath method propyl carbinol, the suitable quantity of water dissolving, last AB-8 macroporous adsorptive resins separates; Collect 30% ethanol elution position, concentrate, go up Sephadex LH-20 methanol-water (1: 1) post wash-out repeatedly; Remove pigment; Concentrate flow point, in methyl alcohol, separate out colourless crystallization, recrystallizing methanol obtains east grass of meadow rue glycosides.Chinese patent 200910312563.3 disclosed " a kind of semiaquilegia root extract "; Adopt bright article or dry product; Extract with extraction solvent; The gained extracting solution obtains semiaquilegia root extract after removing and desolvating, and again extract is carried out SX or column chromatography purification, and prepared semiaquilegia root extract is used for preparation prevention and treatment cataract medicine.The former adopts a large amount of organic solvents and column chromatography repeatedly, and complex process, loss of effective components are big, yield is low, and the production cycle is long; What the latter obtained is crude extract, can not obtain effective monomer component.
Summary of the invention:
The technical problem that the present invention will solve provides a kind of method of from Root of Muskroot-like Semiaquilegia, extracting lattice row wind lactone and east grass of meadow rue glycosides.
From Root of Muskroot-like Semiaquilegia, extract the method for lattice row wind lactone and east grass of meadow rue glycosides, it is characterized in that method steps is: the methanol solution with 70-100% extracts, and filters; Get extracting solution, add and stir decolouring on the diatom, destainer adds the hollow composite package ultrafiltration of molecular weight cut-off 6000-10000; See through the liquid concentrating under reduced pressure, liquid concentrator is used water-dispersion, adds macroporous adsorbent resin column chromatography absorption 1-3 time; After absorption finishes; Use the aqueous ethanol gradient elution, collect the flow point of enrichment lattice row wind lactone and east grass of meadow rue glycosides respectively, concentrating under reduced pressure obtains CE respectively again; Lattice row wind lactone CE and polymeric amide are mixed appearance carry out column chromatography, use the chloroform wash-out earlier, use chloroform-methanol (10: 1) wash-out again, collect elutriant, concentrated crystallization, coarse-grain obtains the pure article of lattice row wind lactone with methyl alcohol-acetone recrystallization; East grass of meadow rue glycosides CE and polymeric amide are mixed appearance oven dry upper prop, with alcohol-water elution, with east grass of meadow rue glycosides flow point concentrating under reduced pressure, leave standstill crystallization, coarse-grain obtains the pure article of east grass of meadow rue glycosides with the chloroform-methanol recrystallization again.
Said process for extracting is Suo Shi extraction, reflux, ultrasonic or microwave-assisted extraction.
Said zeyssatite add-on is the 3-5% of extracting solution total amount.
Among the optional DA201 of said macroporous adsorbent resin type, HPD450, XSD-1, the HPD100 any one.
Said macroporous resin wash-out is earlier with the conventional wash-out impurity of deionized water, uses 20% ethanol, 50% ethanol, 95% ethanol elution more successively, collects flow point that is rich in lattice row wind lactone and the flow point that is rich in east grass of meadow rue glycosides respectively.
Advantage of the present invention is: Root of Muskroot-like Semiaquilegia distributes extensively in China, and is therefore cheap and easy to get; Operation is simple for the inventive method, and employing methyl alcohol is extraction solvent, and extraction yield is high; Concentrate through biofilm filtration, remove carbohydrate content; Utilize polymeric amide to form hydrogen bond, have separating effect preferably with nitro-compound and lactone composition.
Embodiment:
Embodiment 1:
Get Root of Muskroot-like Semiaquilegia 500g and be ground into meal or shave, add 8 times of amount 75% methyl alcohol Suo Shi and extract each 1 hour 2 times; Filter, merging filtrate adds 150g zeyssatite and stirs; Filter, destainer adds the hollow composite package ultrafiltration of molecular weight cut-off 6000-10000, sees through the liquid concentrating under reduced pressure; Liquid concentrator adds appropriate amount of deionized water and disperses, and adds in the DA201 macroporous adsorptive resins to adsorb 2 times, and flow velocity is 0.5BV/h; With deionized water wash-out impurity, use 20% ethanol, 50% ethanol, 95% ethanol elution more successively earlier, collect flow point that is rich in lattice row wind lactone and the flow point that is rich in east grass of meadow rue glycosides respectively; Lattice row wind lactone flow point concentrating under reduced pressure is obtained CE, again CE and an amount of polymeric amide are mixed a kind last column chromatography, use earlier the chloroform wash-out; Use chloroform-methanol (10: 1) wash-out again, collect chloroform-methanol (10: 1) elutriant, concentrate crystallization; The filtering coarse-grain; With methyl alcohol-acetone recrystallization, cryodrying promptly gets the pure article of 144mg lattice row wind lactone with coarse-grain, and measuring its content through the HPLC method is 97.2%; With mixing appearance oven dry upper prop in polymeric amide behind the grass of meadow rue glycosides flow point concentrating under reduced pressure of east, use 40% ethanol elution, collect elutriant; Decompression recycling ethanol; Concentrate and leave standstill crystallization, coarse-grain promptly gets the pure article of 189mg east grass of meadow rue glycosides with the chloroform-methanol recrystallization, and measuring its content through the HPLC method is 96.6%.
Embodiment 2:
Get Root of Muskroot-like Semiaquilegia 1000g and be ground into meal or shave, add 10 times of amount 100% methyl alcohol heating and refluxing extraction 2 times, each 1.5 hours; Filter, merging filtrate adds 750g zeyssatite and stirs; Filter, destainer adds the hollow composite package ultrafiltration of molecular weight cut-off 6000-10000, sees through the liquid concentrating under reduced pressure; Liquid concentrator adds appropriate amount of deionized water and disperses, and adds in the HPD450 macroporous adsorptive resins to adsorb, and flow velocity is 1BV/h; With deionized water wash-out impurity, use 20% ethanol, 50% ethanol, 95% ethanol elution more successively earlier, collect flow point that is rich in lattice row wind lactone and the flow point that is rich in east grass of meadow rue glycosides respectively; Lattice row wind lactone flow point concentrating under reduced pressure is obtained CE, again CE and an amount of polymeric amide are mixed a kind last column chromatography, use earlier the chloroform wash-out; Use chloroform-methanol (10: 1) wash-out again, collect chloroform-methanol (10: 1) elutriant, concentrate crystallization; The filtering coarse-grain; With methyl alcohol-acetone recrystallization, cryodrying promptly gets the pure article of 306mg lattice row wind lactone with coarse-grain, and measuring its content through the HPLC method is 96.2%; With mixing appearance oven dry upper prop in polymeric amide behind the grass of meadow rue glycosides flow point concentrating under reduced pressure of east, use 40% ethanol elution, collect elutriant; Decompression recycling ethanol; Concentrate and leave standstill crystallization, coarse-grain promptly gets the pure article of 483mg east grass of meadow rue glycosides with the chloroform-methanol recrystallization, and measuring its content through the HPLC method is 95.9%.
Embodiment 3:
Get Root of Muskroot-like Semiaquilegia 2kg and be ground into meal or shave, add 15 times of amount 80% methyl alcohol supersound extraction 1 time, extracted 2 hours; Filter, add 680g zeyssatite and stir, filter; Destainer adds the hollow composite package ultrafiltration of molecular weight cut-off 6000-10000, sees through the liquid concentrating under reduced pressure, and liquid concentrator adds appropriate amount of deionized water and disperses; Add in the XSD-1 macroporous adsorptive resins and adsorb 2 times, flow velocity is 0.6BV/h, earlier with deionized water wash-out impurity; Use 20% ethanol, 50% ethanol, 95% ethanol elution more successively, collect flow point that is rich in lattice row wind lactone and the flow point that is rich in east grass of meadow rue glycosides respectively; Lattice row wind lactone flow point concentrating under reduced pressure is obtained CE, again CE and an amount of polymeric amide are mixed a kind last column chromatography, use earlier the chloroform wash-out; Use chloroform-methanol (10: 1) wash-out again, collect chloroform-methanol (10: 1) elutriant, concentrate crystallization; The filtering coarse-grain; With methyl alcohol-acetone recrystallization, cryodrying promptly gets the pure article of 584mg lattice row wind lactone with coarse-grain, and measuring its content through the HPLC method is 95.7%; With mixing appearance oven dry upper prop in polymeric amide behind the grass of meadow rue glycosides flow point concentrating under reduced pressure of east, use 40% ethanol elution, collect elutriant; Decompression recycling ethanol; Concentrate and leave standstill crystallization, coarse-grain promptly gets the pure article of 743mg east grass of meadow rue glycosides with the chloroform-methanol recrystallization, and measuring its content through the HPLC method is 96.3%.
Embodiment 4:
Get Root of Muskroot-like Semiaquilegia 5kg and be ground into meal or shave, add 6 times of amount 70% methyl alcohol microwave-assisted and extract each 0.5 hour 3 times; Filter, merging filtrate adds 2.3kg zeyssatite and stirs; Filter, destainer adds the hollow composite package ultrafiltration of molecular weight cut-off 6000-10000, sees through the liquid concentrating under reduced pressure; Liquid concentrator adds appropriate amount of deionized water and disperses, and adds in the HPD100 macroporous adsorptive resins absorption times 3, and flow velocity is 0.8BV/h; With deionized water wash-out impurity, use 20% ethanol, 50% ethanol, 95% ethanol elution more successively earlier, collect flow point that is rich in lattice row wind lactone and the flow point that is rich in east grass of meadow rue glycosides respectively; Lattice row wind lactone flow point concentrating under reduced pressure is obtained CE, again CE and an amount of polymeric amide are mixed a kind last column chromatography, use earlier the chloroform wash-out; Use chloroform-methanol (10: 1) wash-out again, collect chloroform-methanol (10: 1) elutriant, concentrate crystallization; The filtering coarse-grain; With methyl alcohol-acetone recrystallization, cryodrying promptly gets the pure article of 1.29g lattice row wind lactone with coarse-grain, and measuring its content through the HPLC method is 96.8%; With mixing appearance oven dry upper prop in polymeric amide behind the grass of meadow rue glycosides flow point concentrating under reduced pressure of east, use 40% ethanol elution, collect elutriant; Decompression recycling ethanol; Concentrate and leave standstill crystallization, coarse-grain promptly gets the pure article of 1.86g east grass of meadow rue glycosides with the chloroform-methanol recrystallization, and measuring its content through the HPLC method is 95.4%.
Claims (5)
1. from Root of Muskroot-like Semiaquilegia, extract the method for lattice row wind lactone and east grass of meadow rue glycosides, it is characterized in that method steps is: the methanol solution with 70-100% extracts, and filters; Get extracting solution, add zeyssatite and stir decolouring, destainer adds the hollow composite package ultrafiltration of molecular weight cut-off 6000-10000; See through the liquid concentrating under reduced pressure, liquid concentrator is used water-dispersion, adds macroporous adsorbent resin column chromatography absorption 1-3 time; After absorption finishes; Use the aqueous ethanol gradient elution, collect the flow point of enrichment lattice row wind lactone and Dong Fangtangsong leather glycosides respectively, concentrating under reduced pressure obtains CE respectively again; Lattice row wind lactone CE and polymeric amide are mixed appearance carry out column chromatography, use the chloroform wash-out earlier, use chloroform-methanol (10: 1) wash-out again, collect elutriant, concentrated crystallization, coarse-grain obtains the pure article of lattice row wind lactone with methyl alcohol-acetone recrystallization; East grass of meadow rue glycosides CE and polymeric amide are mixed appearance oven dry upper prop, with alcohol-water elution, with east grass of meadow rue glycosides flow point concentrating under reduced pressure, leave standstill crystallization, coarse-grain obtains the pure article of east grass of meadow rue glycosides with the chloroform-methanol recrystallization again.
2. the method for extraction lattice row wind lactone according to claim 1 and east grass of meadow rue glycosides is characterized in that said process for extracting is Suo Shi extraction, reflux, ultrasonic or microwave-assisted extraction.
3. the method for extraction lattice row wind lactone according to claim 1 and east grass of meadow rue glycosides is characterized in that said zeyssatite add-on is the 3-5% of extracting solution total amount.
4. the method for extraction lattice row wind lactone according to claim 1 and east grass of meadow rue glycosides is characterized in that among the optional DA201 of said macroporous adsorbent resin type, HPD450, XSD-1, the HPD100 any one.
5. the method for extraction lattice row wind lactone according to claim 1 and east grass of meadow rue glycosides; It is characterized in that said macroporous resin wash-out is earlier with the conventional wash-out impurity of deionized water; Use 20% ethanol, 50% ethanol, 95% ethanol elution more successively, collect flow point that is rich in lattice row wind lactone and the flow point that is rich in east grass of meadow rue glycosides respectively.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111077245A (en) * | 2019-12-23 | 2020-04-28 | 广东一方制药有限公司 | UPLC characteristic spectrum establishing method and detection method of radix semiaquilegiae medicinal material |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101773553A (en) * | 2009-12-29 | 2010-07-14 | 汤磊 | Semiaquilegia root extract, preparation method and application thereof |
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2011
- 2011-02-25 CN CN2011100453633A patent/CN102649782A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101773553A (en) * | 2009-12-29 | 2010-07-14 | 汤磊 | Semiaquilegia root extract, preparation method and application thereof |
Non-Patent Citations (2)
| Title |
|---|
| 张洪泉等: "《临床药学基础与应用》", 31 August 2003, article "天然药物的提取与制备工艺研究", pages: 136-137 * |
| 牛锋: "天葵子的化学成分及质量标准研究", 《中国优秀博硕士学位论文全文数据库（博士）医药卫生科技辑》, 15 January 2007 (2007-01-15), pages 057 - 31 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111077245A (en) * | 2019-12-23 | 2020-04-28 | 广东一方制药有限公司 | UPLC characteristic spectrum establishing method and detection method of radix semiaquilegiae medicinal material |
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Application publication date: 20120829 |