CN102204955A - Method for extracting ketone substance and salvianolic acid substance from salvia root simultaneously - Google Patents
Method for extracting ketone substance and salvianolic acid substance from salvia root simultaneously Download PDFInfo
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- CN102204955A CN102204955A CN 201110113893 CN201110113893A CN102204955A CN 102204955 A CN102204955 A CN 102204955A CN 201110113893 CN201110113893 CN 201110113893 CN 201110113893 A CN201110113893 A CN 201110113893A CN 102204955 A CN102204955 A CN 102204955A
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- salvianolic acid
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Abstract
The invention relates to a method for extracting a ketone substance and a salvianolic acid substance from salvia root simultaneously, belonging to a new separation technique. The method provided by the invention is characterized by taking an alcoholic water solution as a solvent, using acid to regulate the pH value of a solution, and extracting the fat-soluble tanshinone substance and the water-soluble salvianolic acid substance simultaneously by metallic ion complexometry by magnesium, calcium and the like. In the concentration process of the solvent, the organic solvent alcohol is distilled off first, and the fat-soluble tanshinone substance is separated out first to obtain the tanshinone substance; and the left water contains the water-soluble salvianolic acid substance, and the water is removed by distillation to obtain the solid containing the salvianolic acid substance. The method has a simple process and low cost.
Description
Technical field
The present invention relates to a kind of method of extracting letones and salvianolic acid class material in the Radix Salviae Miltiorrhizae simultaneously, belong to the isolating technical field of fine chemical product.
Background technology
Radix Salviae Miltiorrhizae bitter in the mouth, little suffering, cold nature are a kind of Chinese medicine with extensive use, be applicable to cardiovascular disease treatment, promote tissue reparation and regeneration, improve the liver microcirculation, external staphylococcus, escherichia coli, degeneration bacillus are had inhibitory action.Effective ingredient in the Radix Salviae Miltiorrhizae mainly is tanshinone material and salvianolic acid class material, and wherein the salvianolic acid B content in Radix Salviae Miltiorrhizae in the salvianolic acid class material is the highest, and effect clearly, is considered to one of main matter of Radix Salviae Miltiorrhizae performance curative effect effect.
At present, the extracting method of above-mentioned two class materials separately carries out mostly, and wherein 95% ethanol extraction is mainly adopted in the extraction of tanshinone material, pure content height, and extraction effect is good, because the tanshinone material is fat-soluble, is dissolved in organic solvent; And salvianolic acid class material extracts the main water extraction that adopts, because salvianolic acid class material is a water solublity.Along with the increase of Radix Salviae Miltiorrhizae class drug dose demand, improve the extracting method of above-mentioned two kinds of materials, the emphasis that the reduction extraction cost has become correlational study.
Summary of the invention
The objective of the invention is to be to provide a kind of method of extracting letones and salvianolic acid class material in the Radix Salviae Miltiorrhizae simultaneously, this method production cost is low, product yield is high, process is pollution-free.
The present invention is achieved by the following technical solutions.Come letones and salvianolic acid class material in the separation and Extraction Radix Salviae Miltiorrhizae with the complexing of metal ion method.It is characterized in that, adopt metal ions such as magnesium, calcium to come complexation tanshinone material, utilize the adjacent diketone structure in the tanshinone material and the performance of complexing of metal ion, increase polarity, thereby can in the lower aqueous solution of pure content, dissolve and be extracted, and, adopt acid to come the regulator solution pH value because metal ion complexation under acid condition is effective; Simultaneously, salvianolic acid class material also can carry out complexing, and pH value can regulate the ionization situation of salvianolic acid class material, and solute effect might as well in the pure water thereby such material is in low the containing of pH value.Therefore, adopt the assisted extraction agent of metal ion to combine, adopt the aqueous solution that contains alcohol, extract fat-soluble tanshinone material and water miscible salvianolic acid class material simultaneously with the pH regulator agent.Then, in the solvent concentration process, organic solvent steams earlier, and fat-soluble tanshinone material is separated out earlier, obtains the tanshinone material; Be the salvianolic acid class material that contains water solublity in the water, distillation is anhydrated, and obtains containing the solid of salvianolic acid class material.
The invention has the advantages that separation efficiency is good, cost is low, and production technology is simple, can not produce adverse effect to human body, animal and environment, can not destroy ecology and environment.
The specific embodiment
Embodiment one
60 ℃ of oven dry of red rooted salvia (measure according to official method in 2005, wherein tanshinone content 0.38%, content of danshinolic acid B 6%), it is standby to cross 40 mesh sieves after pulverizing.Get 100 gram Danshen Roots, the alcoholic solution that adds 8 times of amounts 30%, add 4 gram magnesium chlorides, transfer pH value to 5 with concentrated hydrochloric acid, 1.5 hours after-filtration of heating and refluxing extraction, filtering residue adds the alcoholic solution of 6 times of amounts 30%, adds 2 gram magnesium chlorides, transfer pH value to 5 with concentrated hydrochloric acid, 1.5 hours after-filtration of reheat backflow.Twice filtrate merges, and concentrating under reduced pressure to 2 times volume (2mL/ restrain medical material) filters, and obtains containing tanshinone and seldom measures the red-black colour band viscous solid (obtain 3.6 and restrain the black solid extracts, wherein tanshinone content 6.9%) of salvianolic acid B.Concentrated filtrate is to solid, and vacuum drying obtains containing the solid (obtain 14.7 gram brown solid extracts, wherein content of danshinolic acid B 29.4%) of salvianolic acid B.
Embodiment two
60 ℃ of oven dry of red rooted salvia (measure according to official method in 2005, wherein tanshinone content 0.38%, content of danshinolic acid B 6%), it is standby to cross 40 mesh sieves after pulverizing.Get 100 gram Danshen Roots, the alcoholic solution that adds 8 times of amounts 40%, add 5 gram calcium chloride, transfer pH value 4.5 with concentrated hydrochloric acid, 1.5 hours after-filtration of heating and refluxing extraction, filtering residue adds the alcoholic solution of 6 times of amounts 40%, adds 2 gram calcium chloride, transfer pH value to 4.5 with concentrated hydrochloric acid, 1.5 hours after-filtration of reheat backflow.Twice filtrate merges, and concentrating under reduced pressure to 2 times volume (2mL/ restrain medical material) filters, and obtains containing tanshinone and seldom measures the red-black colour band viscous solid (obtain 4.3 and restrain the black solid extracts, wherein tanshinone content 5.1%) of salvianolic acid B.Concentrated filtrate is to solid, and vacuum drying obtains containing the solid (obtain 14.6 gram brown solid extracts, wherein content of danshinolic acid B 25.4%) of salvianolic acid B.
Embodiment three
60 ℃ of oven dry of red rooted salvia (measure according to official method in 2005, wherein tanshinone content 0.38%, content of danshinolic acid B 6%), it is standby to cross 40 mesh sieves after pulverizing.Get 100 gram Danshen Roots, the alcoholic solution that adds 8 times of amounts 40%, add 4 gram magnesium sulfate, transfer pH value to 4 with concentrated hydrochloric acid, 1.5 hours after-filtration of heating and refluxing extraction, filtering residue adds the alcoholic solution of 6 times of amounts 40%, adds 2 gram magnesium sulfate, transfer pH value to 4 with concentrated hydrochloric acid, 1.5 hours after-filtration of reheat backflow.Twice filtrate merges, and concentrating under reduced pressure to 2 times volume (2mL/ restrain medical material) filters, and obtains containing Tanshinone I I A and seldom measures the red-black colour band viscous solid (obtain 3.2 and restrain the black solid extracts, wherein tanshinone content 7.2%) of salvianolic acid B.Concentrated filtrate is to solid, and vacuum drying obtains containing the solid (obtain 12.7 gram brown solid extracts, wherein content of danshinolic acid B 32.4%) of salvianolic acid B.
Claims (1)
1. method of extracting letones and salvianolic acid class material in the Radix Salviae Miltiorrhizae simultaneously is characterized in that may further comprise the steps:
A, adopting the content of 6～9 times of Danshen Root amounts is 20～50% alcohol solution dipping Danshen Roots, adds 2～6 gram magnesium chloride or calcium chloride, or corresponding sulfate, transfers pH value to 2～6,2～4 hours after-filtration of heating and refluxing extraction with hydrochloric acid or sulphuric acid then;
B, filtering residue adds the alcoholic solution of 3～6 times of amounts 20～50%, adds 1～3 gram magnesium chloride or calcium chloride, or corresponding sulfate, transfers pH value to 2～6,2～4 hours after-filtration of reheat reflux, extract, with hydrochloric acid or sulphuric acid then;
C, twice filtrate merges, concentrating under reduced pressure to 2 times volume (2mL/ restrain medical material), filtration obtains containing tanshinone and seldom measures the red-black colour band viscous solid of salvianolic acid B;
D, concentrated filtrate be to solid, and vacuum drying obtains containing the solid of salvianolic acid B.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201110113893.7A CN102204955B (en) | 2011-05-04 | 2011-05-04 | Method for extracting ketone substance and salvianolic acid substance from salvia root simultaneously |
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| CN201110113893.7A CN102204955B (en) | 2011-05-04 | 2011-05-04 | Method for extracting ketone substance and salvianolic acid substance from salvia root simultaneously |
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| CN102204955A true CN102204955A (en) | 2011-10-05 |
| CN102204955B CN102204955B (en) | 2014-04-23 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015149589A1 (en) * | 2014-04-01 | 2015-10-08 | 中国科学院上海药物研究所 | High-purity magnesium lithospermate b and preparation method therefor |
| CN113694562A (en) * | 2021-09-14 | 2021-11-26 | 山东明仁福瑞达制药股份有限公司 | Traditional Chinese medicine concentrated solution purification device and method |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101401843A (en) * | 2008-11-18 | 2009-04-08 | 阳国平 | Extracting method for active principle of traditional Chinese medicine red sage root |
| CN101757105A (en) * | 2010-02-23 | 2010-06-30 | 广州汉方现代中药研究开发有限公司 | Extraction method capable of enriching fat soluble and water soluble parts of salvia simultaneously |
| CN101863957A (en) * | 2010-07-15 | 2010-10-20 | 三明华健生物工程有限公司 | Method for synchronously extracting tanshinone IIA and salvianolic acid B from danshen root efficiently |
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2011
- 2011-05-04 CN CN201110113893.7A patent/CN102204955B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101401843A (en) * | 2008-11-18 | 2009-04-08 | 阳国平 | Extracting method for active principle of traditional Chinese medicine red sage root |
| CN101757105A (en) * | 2010-02-23 | 2010-06-30 | 广州汉方现代中药研究开发有限公司 | Extraction method capable of enriching fat soluble and water soluble parts of salvia simultaneously |
| CN101863957A (en) * | 2010-07-15 | 2010-10-20 | 三明华健生物工程有限公司 | Method for synchronously extracting tanshinone IIA and salvianolic acid B from danshen root efficiently |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2015149589A1 (en) * | 2014-04-01 | 2015-10-08 | 中国科学院上海药物研究所 | High-purity magnesium lithospermate b and preparation method therefor |
| JP2017510592A (en) * | 2014-04-01 | 2017-04-13 | シャンハイ・インスティチュート・オブ・マテリア・メディカ・チャイニーズ・アカデミー・オブ・サイエンシズＳｈａｎｇｈａｉ Ｉｎｓｔｉｔｕｔｅ Ｏｆ Ｍａｔｅｒｉａ Ｍｅｄｉｃａ，Ｃｈｉｎｅｓｅ Ａｃａｄｅｍｙ Ｏｆ Ｓｃｉｅｎｃｅｓ | High-purity magnesium lithospermate and method for producing the same |
| US10259798B2 (en) * | 2014-04-01 | 2019-04-16 | Shanghai Institute Of Materia Medica Chinese Academy Of Sciences | High-purity magnesium lithospermate B and preparation method therefor |
| CN113694562A (en) * | 2021-09-14 | 2021-11-26 | 山东明仁福瑞达制药股份有限公司 | Traditional Chinese medicine concentrated solution purification device and method |
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| CN102204955B (en) | 2014-04-23 |
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