CN1410423A - Technical method of extracting rutin - Google Patents
Technical method of extracting rutin Download PDFInfo
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- CN1410423A CN1410423A CN 01128909 CN01128909A CN1410423A CN 1410423 A CN1410423 A CN 1410423A CN 01128909 CN01128909 CN 01128909 CN 01128909 A CN01128909 A CN 01128909A CN 1410423 A CN1410423 A CN 1410423A
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Abstract
A process for extracting rutin includes such steps as pulverizing tartavian buckwheat, baking thermal extracting in solvent, filtering to obtain coarse extract, distilling filtrate to recover solvent; dissolving the coarse extract in solvent, depasiting, filtering to obtain rutin extract, thermal extracting in solvent, filtering to obtain coarse rutin, dissolving in solvent, heating while stirring, fitlering, adsorbing the filtrate, eduting, distilling, centrifugal filtering, and baking at under 80 deg.C to obtain the refined product. Its advantages are high output rate and purity, and no environmental pollution.
Description
The invention belongs to the preparation field of medicine, specifically is a kind of processing method of extracting rutin.
Rutin is a flavonoid compound, claims cloud spiceleaf glucoside or vitamin P again.At present, China extracts rutin from woody leguminous plants sophora bud bud (sophora bud), but this method raw material sources difficulty, complex process yields poorly.The report that extracts rutin is also arranged in recent years from bitter buckwheat, is to remove the floating thing of water with being soaked in water after the bitter buckwheat corase grind as CN98112256.6, then with alcohol-pickled, extract, filter, dry rutin.Though this method technology is simple, process recovery ratio is low, poor product quality.
The objective of the invention is to overcome the defective of above-mentioned prior art, be easy to get the product yield height for people provide a kind of raw material, good product purity, production technique low toxicity, safety, the process time is short, non-environmental-pollution, waste residue can be used as the processing method of the extraction rutin of feed or fertilizer.
The objective of the invention is to realize by following technical proposals.
The processing method of extraction rutin of the present invention is:
A: buckwheat powder is broken, dry, then by bitter buckwheat: the part by weight of solvent=1: 6～25 extracted 4～24 hours with stirring solvent under 65～80C, filtered and removed fibrous residue, and the filtrate distillating recovering solvent gets the rutin crude extract; Wherein, solvent is methyl alcohol or ethanol, acetone, formaldehyde;
B: above-mentioned rutin crude extract is pressed bitter buckwheat: the part by weight of solvent=1: 6～30 is removed impurity such as protein and part tannin, pigment with solvent normal-temperature dissolution, precipitation, filtration, and the filtrate distillating recovering solvent gets the rutin extract; Wherein, solvent is Virahol or propyl carbinol, propyl alcohol, isopropylcarbinol, amylalcohol, propylene glycol, butyleneglycol, vinylcarbinol;
C: above-mentioned rutin extract is pressed bitter buckwheat: the part by weight of solvent=1: 6～20 heats extraction 0.5～2 hour with solvent under 65～110C, filters, and the filtrate distillating recovering solvent gets the rutin crude product; Wherein, solvent is trichloromethane or monochloro methane, methylene dichloride, tetracol phenixin, ether, gasoline, sherwood oil, toluene;
D: with above-mentioned rutin crude product by bitter buckwheat: the part by weight of solvent=1: 5～20 is with solvent heated and stirred 0.5～2 hour under 65～95C, and filtered while hot is removed filter residue, filtrate that must be purer; Wherein, solvent is a kind of in ethanol, methyl alcohol, vinyl acetic monomer, methyl-formiate, ethyl formate, methyl acetate, ring ethanol, propyl alcohol, acetate, the formic acid or wherein two kinds, three kinds;
E: above-mentioned filtrate is adsorbed with adsorption column, adsorption column is polyamide column, alumina column, gel column, sephadex column, cellulose powder post, silicagel column, macroporous adsorptive resins, ion exchange resin column, wash post with in ethanol, methyl alcohol, distilled water, the formaldehyde one or both, elutriant reclaims solvent through distilling to concentrate, centrifuging, dry below the 80C the elaboration rutin.
In the such scheme, add filtrate heavy 0.3%～5% gac or diatomite or aluminum oxide or silica gel in the filtrate before adsorbing, to remove impurity such as pigment.
Technique scheme is the contriver gropes the science summing up out repeatedly by long-term practice a technical scheme, raw materials used bitter buckwheat is easy to get, it is grown in high and cold, high altitude localities, has drought-enduring, impoverishment tolerant, characteristics that growth is fast, can grow for 2～4 seasons every year in Aba, Ganzi, the Liangshan Mountain.From bitter buckwheat, extract rutin, can solve and only rely on that sophora bud approach is single, the defective of the contradiction of resource-constrained and the prior art that overcomes.The present invention adopts high-new isolation technique, fully the hydrophilic and hydrophobicity characteristics of five kinds of different solvents of utilization, ten minutes separate rutin effectively from bitter buckwheat, productive rate reaches more than 98.5%, product meets the rutin powder standard of U.S. NF-11 version fully, product purity is greater than 96%, residue is less than 2%, and Quercetin is less than 2%, and red green plain 0.04%.
Solvent for use is energy recovery set usefulness all, treated organic composite fertilizer or the feed of can be used for of bitter buckwheat fibrous residue, and whole industrial production is a green cleaning technology process of typical case.Life cycle of the product only has three days, and production cost is low, production technique low toxicity, safety, non-environmental-pollution.
Be embodiments of the invention below, but the present invention is not limited only to described embodiment.
Embodiment one
A: bitter buckwheat is cleaned, be ground into the length of 2～3mm, the moisture content of oven dry to 6%, then by bitter buckwheat: the part by weight of solvent=1: 6 stirs under 65C with methyl alcohol and extracted in 24 hours, filter and remove fibrous residue, methyl alcohol is reclaimed in distillation, must contain the rutin extract of impurity such as tannin, protein, pigment.Purpose is to remove fiber.
B: with the said extracted thing by bitter buckwheat: the part by weight Virahol normal-temperature dissolution of solvent=1: 6, precipitate 20 minutes after-filtration, impurity such as removal protein and part tannin, pigment.Reclaim Virahol, must contain the rutin extract of impurity such as tannin, pigment.
C: with the said extracted thing by bitter buckwheat: the part by weight of solvent=1: 6 extracted 2 hours under 65C with trichloromethane, filtered, and removed impurity such as tannin, pigment, got the rutin crude product.Reclaim trichloromethane.
D: with above-mentioned rutin crude product by bitter buckwheat: the part by weight of solvent=1: 5 stirred 2 hours filtered while hot, removal filter residue, filtrate that must be purer under 65C with 55: 45 the ethanol and the mixture of vinyl acetic monomer.
E: above-mentioned filtrate is adsorbed, adopt polymeric amide adsorption column absorption rutin.Ethanol with 70% is washed post.Concentrate eluant reclaims ethanol, centrifuging, dry below the 80C the elaboration rutin.
Embodiment two
A: bitter buckwheat is cleaned, be ground into the length of 2～3mm, then by bitter buckwheat: the part by weight of solvent=1: 20 with acetone extraction 12 hours, filters and removes fibrous residue under 80C, reclaims acetone, must contain the rutin extract of impurity such as tannin, protein, pigment.
B: with the said extracted thing by bitter buckwheat: the part by weight propyl carbinol normal-temperature dissolution of solvent=1: 10, precipitate 10 minutes, filtration, impurity such as removal protein and part tannin, pigment.Reclaim propyl carbinol.The rutin extract that must contain impurity such as tannin, pigment.
C: with the said extracted thing by bitter buckwheat: the part by weight of solvent=1: 8 extracted 0.5 hour filtration under 110C with trichloromethane.Remove impurity such as tannin, pigment, get the rutin crude product.Reclaim trichloromethane.
D: with above-mentioned rutin crude product by bitter buckwheat: the part by weight of solvent=1: 6 stirred 0.5 hour filtered while hot, removal filter residue, filtrate that must be purer under 80C with ethanol.
The gac of adding 0.3%, stirring at normal temperature 1 hour leaches gac.
E: above-mentioned filtrate is adsorbed, adopt alumina adsorption post absorption rutin.Wash post with methyl alcohol.Concentrate eluant reclaims solvent, centrifuging, dry under the 80C the elaboration rutin.
Embodiment three
A: bitter buckwheat is cleaned, be ground into the length of 2～3mm, then by bitter buckwheat: the part by weight of solvent=1: 25 extracted 4 hours under 80C with ethanol, filtered and removed fibrous residue, and recovery ethanol must contain the rutin extract of impurity such as tannin, protein, pigment.
B: with the said extracted thing by bitter buckwheat: the part by weight of solvent=1: 30 is with amylalcohol normal-temperature dissolution, precipitation, filters impurity such as removing protein and part tannin, pigment.Reclaim amylalcohol, must contain the rutin extract of impurity such as tannin, pigment.
C: with the said extracted thing by bitter buckwheat: the part by weight of solvent=1: 20 filters impurity such as removing tannin, pigment with methylene dichloride heating and refluxing extraction 1 hour, the rutin crude product.Reclaim methylene dichloride.
D: with above-mentioned rutin crude product by bitter buckwheat: the part by weight of solvent=1: 20 stirred 1 hour filtered while hot, removal filter residue, filtrate that must be purer under 95C with vinyl acetic monomer.
The aciculiform gac of adding 5% in the filtrate, stirring at normal temperature 20 minutes leaches the aciculiform gac.
E: above-mentioned filtrate is adsorbed, adopt silica gel adsorption column absorption rutin.With distillation washing post.Elutriant concentrates, centrifuging, dry under the 80C the elaboration rutin.
Embodiment four
A: bitter buckwheat is cleaned, be ground into the length of 2～3mm, the moisture content of oven dry to 6%, then by bitter buckwheat: the part by weight of solvent=1: 15 under 80C with extraction using alcohol 6 hours, filter and remove fibrous residue, reclaim ethanol (can use repeatedly), must contain the rutin extract of impurity such as tannin, protein, pigment.
B: with the said extracted thing by bitter buckwheat: the part by weight butyleneglycol normal-temperature dissolution of solvent=1: 15, precipitation is filtered impurity such as removal protein and part tannin, pigment.Reclaim butyleneglycol (can use repeatedly), must contain the rutin extract of impurity such as tannin, pigment.
C: with the said extracted thing by bitter buckwheat: the part by weight of solvent=1: 10 extracted 0.5 hour under 100C with sherwood oil, filtered impurity such as removing tannin, pigment, got the rutin crude product.Reclaim sherwood oil (can use repeatedly).
D: with above-mentioned rutin crude product by bitter buckwheat: the part by weight of solvent=1: 10 stirred 1 hour filtered while hot, removal filter residue, filtrate that must be purer under 80C with acetate.
The silica gel of adding 3% in the filtrate, stirring at normal temperature 1 hour leaches silica gel.
E: above-mentioned filtrate is adsorbed, adopt macroporous resin adsorption post absorption rutin.Ethanol with 70% is washed post.Concentrate eluant reclaims solvent, centrifuging, dry under the 80C the elaboration rutin.
Claims (2)
1. processing method of extracting rutin is characterized in that processing step is:
A: buckwheat powder is broken, oven dry, then by bitter buckwheat: the part by weight of solvent=1: 6～25 extracted 4～24 hours with stirring solvent under 65～80C, filtered, and the filtrate distillating recovering solvent gets the rutin crude extract; Wherein, solvent is methyl alcohol or ethanol, acetone, formaldehyde;
B: above-mentioned rutin crude extract is pressed bitter buckwheat: the part by weight of solvent=1: 6～30 solvent normal-temperature dissolution, precipitation, filtration, the filtrate distillating recovering solvent gets the rutin extract; Wherein, solvent is Virahol or propyl carbinol, propyl alcohol, isopropylcarbinol, amylalcohol, propylene glycol, butyleneglycol, vinylcarbinol;
C: above-mentioned rutin extract is pressed bitter buckwheat: the part by weight of solvent=1: 6～20 heats extraction 0.5～2 hour with solvent under 65～110C, filters, and the filtrate distillating recovering solvent gets the rutin crude product; Wherein, solvent is trichloromethane or monochloro methane, methylene dichloride, tetracol phenixin, ether, gasoline, sherwood oil, toluene;
D: with above-mentioned rutin crude product by bitter buckwheat: the part by weight of solvent=1: 5～20 is with solvent heated and stirred 0.5～2 hour under 65～95C, and filtered while hot is removed filter residue, filtrate that must be purer; Wherein, solvent is a kind of in ethanol, methyl alcohol, vinyl acetic monomer, methyl-formiate, ethyl formate, methyl acetate, ring ethanol, propyl alcohol, acetate, the formic acid or wherein two kinds, three kinds;
E: above-mentioned filtrate is adsorbed with adsorption column, adsorption column is polyamide column, alumina column, gel column, sephadex column, cellulose powder post, silicagel column, macroporous adsorptive resins, ion exchange resin column, wash post with in ethanol, methyl alcohol, distilled water, the formaldehyde one or both, elutriant reclaims solvent through distilling to concentrate, centrifuging, dry below the 80C the elaboration rutin.
2. the processing method of extraction according to claim 1 rutin adds filtrate heavy 0.3%～5% gac or diatomite or aluminum oxide or silica gel in the filtrate before it is characterized in that adsorbing.
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| CNB011289090A CN1151142C (en) | 2001-09-28 | 2001-09-28 | Technical method of extracting rutin |
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| CNB011289090A CN1151142C (en) | 2001-09-28 | 2001-09-28 | Technical method of extracting rutin |
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Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324040C (en) * | 2003-12-26 | 2007-07-04 | 山西省风陵渡开发区众力投资发展有限公司 | Medicament for treating diabetes, diabetes complication, its preparation and novel use |
| CN101972311A (en) * | 2010-11-02 | 2011-02-16 | 浙江大学 | Method for purifying Tartary buckwheat flavone |
| CN102180921A (en) * | 2011-03-25 | 2011-09-14 | 宁夏大学 | Method for extracting high-purity rutin from boxthorn leaves |
| CN102731593A (en) * | 2011-04-02 | 2012-10-17 | 中国科学院兰州化学物理研究所 | Method for extracting rutin from tartary buckwheat |
| CN103012508A (en) * | 2011-09-26 | 2013-04-03 | 阅微生物技术（上海）有限公司 | Tartary buckwheat phenylpropanoid glycoside compound and preparation method and application thereof |
| CN103040951A (en) * | 2012-09-07 | 2013-04-17 | 赵立地 | Method for extracting buckwheat flavonoids |
| CN103059081A (en) * | 2012-12-31 | 2013-04-24 | 宁波泰新生物科技有限公司 | Method for extracting quercetin-3-O-rutinose from taxus mairei leaves |
| CN103570662A (en) * | 2013-11-19 | 2014-02-12 | 东南大学 | Preparation method of high-purity rutin |
| CN103833808A (en) * | 2013-12-03 | 2014-06-04 | 西安应化生物技术有限公司 | Method for extraction separation of rutin of tartary buckwheat |
| CN104151380A (en) * | 2014-06-22 | 2014-11-19 | 北京安德益源生物科技有限公司 | Preparation method of high-purity rutin |
| CN104667571A (en) * | 2015-02-06 | 2015-06-03 | 徐大鹏 | Rutin extraction and leaching equipment |
| CN105582062A (en) * | 2016-01-15 | 2016-05-18 | 中国农业科学院作物科学研究所 | Tartary buckwheat bran extract and externally-used preparation used for skin and containing extract |
| CN105859701A (en) * | 2016-05-13 | 2016-08-17 | 南京财经大学 | Method for extracting and separating flavonoid monomeric substances from common buckwheat husks |
| CN106928290A (en) * | 2017-03-02 | 2017-07-07 | 河南师范大学 | A kind of preparation method of high content rutin |
| CN107432304A (en) * | 2016-06-16 | 2017-12-05 | 西昌学院 | The processing method of buckwheat potato cake |
| CN107434816A (en) * | 2016-05-25 | 2017-12-05 | 辽宁药联制药有限公司 | One kind extracts rutin method from Ilex Latifolia Thunb |
| CN111587883A (en) * | 2020-06-04 | 2020-08-28 | 兰州大学 | Plant pesticide and preparation method and use method thereof |
-
2001
- 2001-09-28 CN CNB011289090A patent/CN1151142C/en not_active Expired - Fee Related
Cited By (22)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1324040C (en) * | 2003-12-26 | 2007-07-04 | 山西省风陵渡开发区众力投资发展有限公司 | Medicament for treating diabetes, diabetes complication, its preparation and novel use |
| CN101972311A (en) * | 2010-11-02 | 2011-02-16 | 浙江大学 | Method for purifying Tartary buckwheat flavone |
| CN102180921A (en) * | 2011-03-25 | 2011-09-14 | 宁夏大学 | Method for extracting high-purity rutin from boxthorn leaves |
| CN102180921B (en) * | 2011-03-25 | 2014-02-12 | 宁夏大学 | Method for extracting high-purity rutin from boxthorn leaves |
| CN102731593A (en) * | 2011-04-02 | 2012-10-17 | 中国科学院兰州化学物理研究所 | Method for extracting rutin from tartary buckwheat |
| CN103012508A (en) * | 2011-09-26 | 2013-04-03 | 阅微生物技术（上海）有限公司 | Tartary buckwheat phenylpropanoid glycoside compound and preparation method and application thereof |
| CN103012508B (en) * | 2011-09-26 | 2015-08-26 | 阅微生物技术（上海）有限公司 | Radix Et Rhizoma Fagopyri Tatarici Phenylpropanoid Glycosides glycosides compound and its production and use |
| CN103040951A (en) * | 2012-09-07 | 2013-04-17 | 赵立地 | Method for extracting buckwheat flavonoids |
| CN103059081B (en) * | 2012-12-31 | 2015-06-24 | 宁波泰新生物科技有限公司 | Method for extracting quercetin-3-O-rutinose from taxus mairei leaves |
| CN103059081A (en) * | 2012-12-31 | 2013-04-24 | 宁波泰新生物科技有限公司 | Method for extracting quercetin-3-O-rutinose from taxus mairei leaves |
| CN103570662A (en) * | 2013-11-19 | 2014-02-12 | 东南大学 | Preparation method of high-purity rutin |
| CN103833808A (en) * | 2013-12-03 | 2014-06-04 | 西安应化生物技术有限公司 | Method for extraction separation of rutin of tartary buckwheat |
| CN104151380A (en) * | 2014-06-22 | 2014-11-19 | 北京安德益源生物科技有限公司 | Preparation method of high-purity rutin |
| CN104667571A (en) * | 2015-02-06 | 2015-06-03 | 徐大鹏 | Rutin extraction and leaching equipment |
| CN105582062A (en) * | 2016-01-15 | 2016-05-18 | 中国农业科学院作物科学研究所 | Tartary buckwheat bran extract and externally-used preparation used for skin and containing extract |
| CN105859701A (en) * | 2016-05-13 | 2016-08-17 | 南京财经大学 | Method for extracting and separating flavonoid monomeric substances from common buckwheat husks |
| CN105859701B (en) * | 2016-05-13 | 2019-04-19 | 南京财经大学 | A method of extracting separating flavone monomeric substance from sweet tea buckwheat shell |
| CN107434816A (en) * | 2016-05-25 | 2017-12-05 | 辽宁药联制药有限公司 | One kind extracts rutin method from Ilex Latifolia Thunb |
| CN107432304A (en) * | 2016-06-16 | 2017-12-05 | 西昌学院 | The processing method of buckwheat potato cake |
| CN106928290A (en) * | 2017-03-02 | 2017-07-07 | 河南师范大学 | A kind of preparation method of high content rutin |
| CN106928290B (en) * | 2017-03-02 | 2020-06-05 | 河南师范大学 | Preparation method of high-content rutin |
| CN111587883A (en) * | 2020-06-04 | 2020-08-28 | 兰州大学 | Plant pesticide and preparation method and use method thereof |
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