CN1312166C - Refining method of raising chrysanthemum total flavone content - Google Patents
Refining method of raising chrysanthemum total flavone content Download PDFInfo
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- CN1312166C CN1312166C CNB031529720A CN03152972A CN1312166C CN 1312166 C CN1312166 C CN 1312166C CN B031529720 A CNB031529720 A CN B031529720A CN 03152972 A CN03152972 A CN 03152972A CN 1312166 C CN1312166 C CN 1312166C
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- chrysanthemum
- total flavone
- macroporous resin
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- flavone content
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Abstract
The present invention relates to a refining method for raising chrysanthemum total flavone content, which comprises the steps of crushing chrysanthemum, extracting solvents, separating and recovering the solvents and concentrating to obtain a thick paste. The refining method comprises the steps that the thick paste is absorbed by macroporous resin, eluted and separated; then, alcohol with the concentration of more than 50% desorbes the thick paste; finally, the solvents are recovered, dried and crushed to obtain extract powder with more than 51% of chrysanthemum total flavone content so that various medicinal preparations can be developed and made from the extract powder. The present invention has the advantages of simple operation and high safety and is suitable for industrial production.
Description
One, technical field
The present invention relates to a kind ofly in herbal medicine, extract and the method for refining activeconstituents specifically a kind of process for purification that improves chrysanthemum total flavone content.
Two, background technology
Chrysanthemum mainly contains multiple compositions such as volatile oil, flavonoid, amino acid, trace element, wherein, flavonoid compound mainly contains flavones and glucosides (as luteolin-7-O-glycoside, apigenin-7-O-glycoside, Acacia-7-O-glycoside) thereof such as luteolin, baicaline, Quercetin, robinin, is generically and collectively referred to as chrysanthemum total flavone.Total flavones has stronger physiologically active in the chrysanthemum, can expand coronary vasodilator, increase coronary flow, also is the main effective constituent of chrysanthemum treatment hypertension and coronary heart disease.
About the method for in chrysanthemum, extracting chrysanthemum total flavone on the professional journals of medicine, medicinal material, field of food and the institute of some universities and colleges newspaper (journal) go up by research widely and report, conclusion is got up to have temperature to soak method, decocting method, is added alkali extraction, supersonic method, alcohol extracting method etc., wherein based on alcohol extracting method.
CN 1150027A discloses a kind of method of extracting available composition of chrysanthemum flower, with under 50～70 ℃ of conditions, extracting 3～3.5 hours after 55～75% the ethanol preimpregnation, with twice of extraction using alcohol, at last once with distilled water extraction, merge and obtain concentrated solution after No. three extracting solutions are sloughed ethanol, chrysanthemum total flavone contains quantity not sufficient 1% in concentrated solution, even further be concentrated into medicinal extract, content of total flavone also can not surpass 5%.
Chrysanthemum total flavone content in extract is low excessively, does not meet the requirement of the modernization of Chinese medicine, and being unfavorable for developing with the chrysanthemum total flavone is the pharmaceutical preparation of main component.
Three, summary of the invention
The present content of various extracting method chrysanthemum total flavones in extract is generally on the low side, and task of the present invention is to increase substantially the content of chrysanthemum total flavone in extract, makes it greater than 51%.
Technical scheme of the present invention comprises that chrysanthemum powder is broken into meal, with refluxing extraction after the solvent preimpregnation, separate and obtain extracting solution, slough solvent and be condensed into thick paste after merging the several times extracting solution, put it briefly, present method comprises the chrysanthemum pulverizing, solvent extraction, through separating, reclaim solvent, concentrate and obtain thick paste, it is characterized in that resulting thick paste macroporous resin adsorption, the ethanol elution of elder generation's water and lower concentration, separate, obtain alcohol extract with the alcohol desorption more than 50% then, slough ethanol and dry at last, pulverizing obtains powdered extract, and the content of chrysanthemum total flavone is greater than 51% in this extract.
Described macroporous resin can be macroporous resins such as AB-8 type, HPD type or D type.
Advantage of the present invention and positively effect:
1. the present invention is through abundant extraction, purifying process, and it is tall and big in 51% that chrysanthemum total flavone accounts for the content of general extractive, can develop and make various pharmaceutical preparations.
2. easy and simple to handle, the safety of the present invention is fit to suitability for industrialized production.
Four, embodiment
Non-limiting examples of the present invention is described below:
1. get the chrysanthemum meal, 70～80% alcohol immersion 1 hour, water-bath refluxes three times then, for the first time, and 10～15 times of amount ethanol, refluxed 1.5 hours: for the second time, 5～7 times of amount ethanol refluxed 1.5 hours; For the third time, 3～4 times of amount ethanol refluxed 1 hour, poured in the medicinal material that next time extracts.Merge first and second extracting solution, reclaim solvent, be condensed into thick, last D
101The type macroporous resin column, water is eluted to sugar-free, wash 3 macroporous resin volumes (hydrochloric acid magnesium powder reaction negative) with 10% ethanol again, wash 3 macroporous resin volumes (hydrochloric acid magnesium powder reacting positive) with 60% ethanol then, collect stream part, use 95% alcohol flushing (hydrochloric acid magnesium powder reaction negative) at last, it is colourless to be washed till effluent liquid, and 60% ethanol part reclaims ethanol, get medicinal extract, 60 ℃ of dryings of vacuum 24 hours get drying solid, are ground into fine powder, promptly get the chrysanthemum total flavone extract, after testing chrysanthemum total flavone content 64% in the extract.Measuring method: with luteolin-7-O-glycoside standard substance is contrast, presses the determined by ultraviolet spectrophotometry optical density, calculates content of total flavone.Down together.
2. get the chrysanthemum meal, add 65% ethanol preimpregnation, ultrasonic extraction 2 times, the 45 minutes, 12 times amount reclaims ethanol and becomes thick paste, last HPD500 type macroporous resin column, successively with water elution to sugar, 10% ethanol elution 3 times, 55% ethanol elution (hydrochloric acid magnesium powder reacting positive), the stream part of collecting 55% ethanol elution, recovery ethanol, vacuum-drying medicinal extract gets finished product, after testing chrysanthemum total flavone content 55% in the extract.
3. get the chrysanthemum meal, add the water preimpregnation, extract 2 times, each 1.5 hours, 10 times water gagings, concentrated extracting solution, last HPD400 type macroporous resin column, successively with water elution to sugar-free, 10% ethanol is washed 3 macroporous resin volumes (hydrochloric acid magnesium powder reaction negative), 50% ethanol is washed 4 macroporous resin volumes (hydrochloric acid magnesium powder reacting positive), collect stream part, back it is colourless to be washed till effluent liquid with 95% alcohol flushing (hydrochloric acid magnesium powder reaction negative), and stream part is through reclaiming ethanol, dry finished product, the chrysanthemum total flavone content 51% in the extract after testing of getting.
4. get the chrysanthemum meal, 95% ethanol preimpregnation, refluxing extraction 3 times, each 10 times of amounts, 40 minutes, concentrated extracting solution, last AB-8 type macroporous resin column, successively with water elution to sugar-free, 10% ethanol is washed 3 macroporous resin volumes (hydrochloric acid magnesium powder reaction negative), 70% ethanol is washed 3 macroporous resin volumes (hydrochloric acid magnesium powder reacting positive), collects stream part, and is back with 95% alcohol flushing (hydrochloric acid magnesium powder reaction negative), it is colourless to be washed till effluent liquid, stream part recovery ethanol, drying records extractive total flavone content 55%.
5. get the chrysanthemum meal, 55% ethanol preimpregnation, refluxing extraction 2 times, each 10 times of amounts, 1 hour, concentrated extracting solution, last HPD600 type macroporous resin column, successively with water elution to sugar-free, 10% ethanol is washed 3 macroporous resin volumes (hydrochloric acid magnesium powder reaction negative), 60% ethanol is washed 3 macroporous resin volumes (hydrochloric acid magnesium powder reacting positive), collects stream part, and is back with 95% alcohol flushing (hydrochloric acid magnesium powder reaction negative), it is colourless to be washed till effluent liquid, stream part recovery ethanol, drying records extractive total flavone content and reaches 64%.
Claims (3)
1, a kind of process for purification that improves chrysanthemum total flavone content, comprise that chrysanthemum is pulverized, solvent extraction, through separating, reclaim solvent, the concentrated thick paste that obtains, it is characterized in that: described thick paste macroporous resin adsorption, the elder generation water with 10% ethanol elution, separate, use the alcohol desorption of 55%～60% concentration then, obtain powdered extract after reclaim solvent, drying, pulverizing.
2, process for purification according to claim 1 is characterized in that: described macroporous resin can be AB-8 type or HPD type or D type macroporous resin.
3, process for purification according to claim 1 and 2 is characterized in that: described macroporous resin is a D type macroporous resin.
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| CNB031529720A CN1312166C (en) | 2003-09-04 | 2003-09-04 | Refining method of raising chrysanthemum total flavone content |
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| CNB031529720A CN1312166C (en) | 2003-09-04 | 2003-09-04 | Refining method of raising chrysanthemum total flavone content |
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| CN1590397A CN1590397A (en) | 2005-03-09 |
| CN1312166C true CN1312166C (en) | 2007-04-25 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101167775B (en) * | 2006-10-27 | 2011-01-12 | 郭颂 | Method for extracting chrysanthemum total flavone |
| CN102188469A (en) * | 2011-05-27 | 2011-09-21 | 河南大学 | Chrysanthemum morifolium extractive with live protection function, extraction method and applications thereof |
| CN107569524A (en) * | 2016-11-21 | 2018-01-12 | 广西大学 | A kind of method of ethanol refluxing process extraction chrysanthemum total flavone |
| CN106511163B (en) * | 2016-11-24 | 2019-12-17 | 江西草珊瑚口腔护理用品有限公司 | Chrysanthemum salt, chrysanthemum salt toothpaste containing chrysanthemum salt and preparation method of chrysanthemum salt toothpaste |
| CN114681501A (en) * | 2022-04-12 | 2022-07-01 | 陈湘 | Chrysanthemum extract with contraceptive effect and plant contraceptive thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1460678A (en) * | 2003-06-04 | 2003-12-10 | 浙江现代中药与天然药物研究院有限公司 | Chrysanthemum total flavone resin purification method |
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Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1460678A (en) * | 2003-06-04 | 2003-12-10 | 浙江现代中药与天然药物研究院有限公司 | Chrysanthemum total flavone resin purification method |
Non-Patent Citations (6)
| Title |
|---|
| AB-8大孔吸附树脂分离长瓣金莲花总黄酮 林秋凤等，暨南大学学报(自然科学版)，第24卷第1期 2003 * |
| AB-8大孔吸附树脂分离长瓣金莲花总黄酮 林秋凤等，暨南大学学报(自然科学版)，第24卷第1期 2003;滁菊花总黄酮类化学成分的分离与鉴定 贾凌云等，中国药物化学杂志，第13卷第3期 2003;菊花总黄酮类物质提取方法的研究 丁利君等，食品工业科技，第23卷第2期 2002;菊花总黄酮的提取工艺的优化 胡春，广州食品工业科技，第12卷第2期 1996;应用大孔吸附树脂吸附分离技术制备蒲黄总黄酮的研究 刘斌等，北京中医药大学学报，第25卷第4期 2002 * |
| 应用大孔吸附树脂吸附分离技术制备蒲黄总黄酮的研究 刘斌等，北京中医药大学学报，第25卷第4期 2002 * |
| 滁菊花总黄酮类化学成分的分离与鉴定 贾凌云等，中国药物化学杂志，第13卷第3期 2003 * |
| 菊花总黄酮的提取工艺的优化 胡春，广州食品工业科技，第12卷第2期 1996 * |
| 菊花总黄酮类物质提取方法的研究 丁利君等，食品工业科技，第23卷第2期 2002 * |
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