CN1616402A - Method for extracting and separating chlorogenic acid - Google Patents
Method for extracting and separating chlorogenic acid Download PDFInfo
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- CN1616402A CN1616402A CN 200310111180 CN200310111180A CN1616402A CN 1616402 A CN1616402 A CN 1616402A CN 200310111180 CN200310111180 CN 200310111180 CN 200310111180 A CN200310111180 A CN 200310111180A CN 1616402 A CN1616402 A CN 1616402A
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- chlorogenic acid
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Abstract
The process of extracting, separating and purifying chlorogenic acid from eucommia leaf and Acertruncatum Bunge leaf includes solvent leaching, resin adsorption, extraction, drying, crystallization and other steps. Compared with available technology, the present invention has the advantages of simple process, low production cost, high product quality, high utility, product purity over 95 %, etc. and the process has passed in industrial test.
Description
Technical field: the present invention is a kind of method of chlorogenic acid extraction separation, relates to the method for chlorogenic acid extracting from plant, special method from Folium Eucommiae and acer truncatum leaf extraction separation chlorogenic acid.
Background technology: at present chlorogenic acid extracting mainly is to be raw material with Japanese Honeysuckle and coffee berry, and both raw materials itself are worth costliness.Also there is the report can be, but the suitability for industrialized production report is not arranged from Folium Eucommiae and acer truncatum leaf extraction separation chlorogenic acid, used complex process, and can't commercial application.
Summary of the invention: the objective of the invention is to: provide a kind of from leaf the method for extraction separation chlorogenic acid, its technology is succinct, the product purity height, production cost is low, is applicable to suitability for industrialized production.The present invention is achieved in that steps such as comprising solvent extraction, resin impurity elimination, resin absorption, extractive crystallization: use high levels of organic solvents, as hydrophilic solvents such as ethanol, acetone, low temperature leaches composition, solvent for use should be lower boiling, easily reclaims hydrophilic solvent, leach liquor carries out selective adsorption and separates by adsorption column.The resin pillar is seen through and the collection of lower concentration elutriant, wherein be rich in the chlorogenic acid component, contain chlorogenic acid, regulate pH value,, the chlorogenic acid component is adsorbed on the resin, wash and be buckled with diluted acid wash-out chlorogenic acid by the polar resin post to after dividing leach liquor to reclaim solvent.Behind the concentrating under reduced pressure, regulate pH value, with the ethyl acetate extraction, ethyl acetate layer recovery solvent gets the chlorogenic acid crude product, and the thick end of crude product chlorogenic acid dissolve with methanol solution filters, and reclaims methyl alcohol, and water recrystallization, vacuum-drying get chlorogenic acid.Specifically:
(1) plant material is ground into meal, leaches with high levels of organic solvents immersion, stirring, insulation, and filtered liquid reclaims, and is dissolved in water, and uses ultrafiltration membrane treatment, gets transparent filtrate.
(2) filtrate has the chromocor compound characteristic reaction to stop by the resin column of adsorption stuffing is housed up to effluent liquid.Collect effluent liquid, towards Xian's resin column, do not stop, collecting rare machine solvent streams fluid to there being the reaction of chlorogenic acid compound characteristic with rare machine solution.
(3) concentrated solution has the reaction of chlorogenic acid compound characteristic to stop in effluent liquid by the exchange column of polar resin is housed.The washing resin filler is to colourless.Do not stop to there being the reaction of chlorogenic acid compound characteristic with diluted acid solvent elution chlorogenic acid.Collect chlorogenic acid component elutriant.
(4) concentrate eluant is regulated pH value to neutral.Use ethyl acetate extraction, organic phase is concentrated into paste, adds diatomite, stirs powdering.Use dissolve with methanol, filter, filtrate is reclaimed methyl alcohol.Get the crude product chlorogenic acid.
(5) crude product chlorogenic acid water recrystallization, vacuum-drying gets chlorogenic acid.
The present invention compared with prior art has characteristics such as technology is simple, manufacturing cost is low, good product quality, yield height, adaptation industrialization production, and product purity is more than 95%, and the present invention tests by suitability for industrialized production.
Embodiments of the invention:
(1) gets at the bottom of May bark of eucommia leaf 1000 grams that dry in the shade, be ground into meal.With 10 liters of immersions of 95% ethanol, heat up 60 ℃, stir and extracted 30 minutes, filter.Filtrate recycling ethanol adds 200 milliliters in water, uses ultrafiltration membrane treatment, gets 150 milliliters of ultrafiltrateds.
(2) filtrate is passed through 20 * 100 chromatography columns, interior dress polymeric amide PA6 particle, and size is 60 orders, collects effluent liquid.Effluent liquid stops to go up sample when the flavones color reaction is arranged, with 200 milliliters of cleanings of clear water, collect scavenging solution, use 10% ethanolic soln wash-out again, no chlorogenic acid component in effluent liquid is collected effluent liquid, effluent liquid and scavenging solution are mixed, be evaporated to no ethanol flavor, get 850 milliliters of solution.
(3) 20 * 100 resin columns that 330 polar resin fillers are housed that above-mentioned gained solution is finished by pre-treatment detect effluent liquid, to there being the chlorogenic acid characteristic reaction to end.Wash resin with water to colourless, being eluted to effluent liquid with the 0.1R hydrochloric acid soln does not more only have the chlorogenic acid characteristic reaction.Collect about 820 milliliters of elutriant and elutriant, vacuum decompression to 500 milliliter.
(4) adjust above-mentioned concentrated solution to PH6-7, with 1: 1 volume ratio ethyl acetate extraction three times, ethyl acetate layer is concentrated, and vacuum is recycled to paste, and add 50 and restrain diatomite, after mixing, the vacuum-drying powdering.Extract diatomite in powder with 200 ml methanol, filter, reclaim methyl alcohol, get 30 gram crude product chlorogenic acids, content is 86%.
(5) crude product chlorogenic acid 500 ml waters are warming up to 50 ℃ of stirring and dissolving, leave standstill, recrystallization filter the chlorogenic acid high purity product.Crystallization again after filtrate concentrates, altogether 21 gram chlorogenic acids, purity is 98.8%.
Embodiments of the invention 2:
(1) gets at the bottom of October acer truncatum leaf 1000 grams that dry in the shade, be ground into fine powder.With 10 liters of immersions of 95% ethanol, heat up 60 ℃, stir and extracted 30 minutes, filter.Filtrate recycling ethanol adds 200 milliliters in water, uses ultrafiltration membrane treatment, gets 120 milliliters of ultrafiltrateds.
(2) filtrate is passed through 20 * 100 chromatography columns, interior dress polymeric amide PA6 particle, and size is 60 orders, collects effluent liquid.Effluent liquid stops to go up sample when the flavones color reaction is arranged, with 200 milliliters of cleanings of clear water, collect scavenging solution, use 10% ethanolic soln wash-out again, no chlorogenic acid component in effluent liquid is collected effluent liquid, effluent liquid and scavenging solution are mixed, be evaporated to no ethanol flavor, get 800 milliliters of solution.
(3) 20 * 100 resin columns that 330 polar resin fillers are housed that above-mentioned gained solution is finished by pre-treatment detect effluent liquid, to there being the chlorogenic acid characteristic reaction to end.Wash resin with water to colourless, being eluted to effluent liquid with the 0.1N hydrochloric acid soln does not more only have the chlorogenic acid characteristic reaction.Collect about 900 milliliters of elutriant and elutriant, vacuum decompression to 600 milliliter.
(4) adjust above-mentioned concentrated solution to PH6-7, with 1: 1 volume ratio ethyl acetate extraction three times, ethyl acetate is strange to be concentrated, and vacuum is recycled to paste, and add 80 and restrain diatomite, after mixing, the vacuum-drying powdering.Extract diatomite in powder with 400 ml methanol, filter, reclaim methyl alcohol, get the thick gram of 50 grams crude product chlorogenic acid, content is 85%.
(5) crude product chlorogenic acid 800 ml waters are warming up to 50 ℃ of stirring and dissolving, leave standstill, recrystallization filter the chlorogenic acid high purity product.Crystallization again after filtrate concentrates, altogether 34 gram chlorogenic acids, purity is 98.5%.
Claims (1)
1, a kind of method of chlorogenic acid extraction separation, comprise solvent extraction, resin absorption, extraction, steps such as crystallizing and drying, it is characterized in that: use high levels of organic solvents, as ethanol, hydrophilic solvents such as acetone, low temperature leaches composition, solvent for use should be lower boiling, easily reclaim hydrophilic solvent, leach liquor carries out selective adsorption and separates by adsorption column, the resin pillar is seen through and the collection of lower concentration elutriant, wherein be rich in the chlorogenic acid component, contain chlorogenic acid, regulate pH value to after dividing leach liquor to reclaim solvent, by the polar resin post, the chlorogenic acid component is adsorbed on the resin, and washing is buckled with diluted acid wash-out chlorogenic acid, behind the concentrating under reduced pressure, the regulator solution pH value, use ethyl acetate extraction, ethyl acetate layer reclaims solvent and gets the chlorogenic acid crude product, the thick end of crude product chlorogenic acid dissolve with methanol solution, filter, reclaim methyl alcohol, the water recrystallization, vacuum-drying gets chlorogenic acid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111180 CN1616402A (en) | 2003-12-12 | 2003-12-12 | Method for extracting and separating chlorogenic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200310111180 CN1616402A (en) | 2003-12-12 | 2003-12-12 | Method for extracting and separating chlorogenic acid |
Publications (1)
| Publication Number | Publication Date |
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| CN1616402A true CN1616402A (en) | 2005-05-18 |
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| CN 200310111180 Pending CN1616402A (en) | 2003-12-12 | 2003-12-12 | Method for extracting and separating chlorogenic acid |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974527B (en) * | 2006-12-01 | 2010-06-23 | 广州汉方现代中药研究开发有限公司 | Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf |
| CN101805261A (en) * | 2010-03-26 | 2010-08-18 | 汉中天然谷生物科技有限公司 | Method for preparing competitive product of chlorogenic acid by folium cortex eucommiae |
| CN101935278A (en) * | 2009-06-11 | 2011-01-05 | 周大捷 | Method for extracting, separating and purifying chlorogenic acid through folium cortex eucommiae |
| CN101941908A (en) * | 2010-09-10 | 2011-01-12 | 武汉巨惠绿色产业发展有限公司 | Method for preparing and partially-synthesizing chlorogenic acid from processing residual liquid of aqua lonicerae foliae |
| CN101602668B (en) * | 2009-07-13 | 2012-06-27 | 江西省科学院应用化学研究所 | Method for extracting chlorogenic acid |
| CN101726560B (en) * | 2008-10-10 | 2013-03-27 | 中国科学院沈阳应用生态研究所 | Method for measuring nutrient concentration of leaves |
| CN103232346A (en) * | 2013-04-06 | 2013-08-07 | 西安宏冠生物科技有限公司 | Production process for extraction of chlorogenic acid from green coffee bean |
| CN105960171A (en) * | 2014-06-13 | 2016-09-21 | 帕万·库马·戈埃尔 | Green coffee bean extract and method thereof |
| JP2017533230A (en) * | 2014-11-26 | 2017-11-09 | スーチョアン チウチャン バイオロジカル サイエンス アンド テクノロジー カンパニー リミテッド | Method for preparing medicinal chlorogenic acid |
| CN107501094A (en) * | 2017-07-26 | 2017-12-22 | 天津泽达天健科技有限公司 | A kind of preparation method of high-purity chlorogenic acid |
| CN107879937A (en) * | 2017-10-24 | 2018-04-06 | 四川九章生物科技有限公司 | A kind of new crystal of chlorogenic acid and preparation method thereof |
| CN114478247A (en) * | 2022-03-01 | 2022-05-13 | 贵州两山康瑞食品检测科技有限公司 | Method for extracting, separating and purifying chlorogenic acid of acer truncatum leaves |
-
2003
- 2003-12-12 CN CN 200310111180 patent/CN1616402A/en active Pending
Cited By (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1974527B (en) * | 2006-12-01 | 2010-06-23 | 广州汉方现代中药研究开发有限公司 | Process of preparing high purity chlorogenic acid and flavonid with eucommia leaf |
| CN101726560B (en) * | 2008-10-10 | 2013-03-27 | 中国科学院沈阳应用生态研究所 | Method for measuring nutrient concentration of leaves |
| CN101935278A (en) * | 2009-06-11 | 2011-01-05 | 周大捷 | Method for extracting, separating and purifying chlorogenic acid through folium cortex eucommiae |
| CN101602668B (en) * | 2009-07-13 | 2012-06-27 | 江西省科学院应用化学研究所 | Method for extracting chlorogenic acid |
| CN101805261A (en) * | 2010-03-26 | 2010-08-18 | 汉中天然谷生物科技有限公司 | Method for preparing competitive product of chlorogenic acid by folium cortex eucommiae |
| CN101941908A (en) * | 2010-09-10 | 2011-01-12 | 武汉巨惠绿色产业发展有限公司 | Method for preparing and partially-synthesizing chlorogenic acid from processing residual liquid of aqua lonicerae foliae |
| CN103232346A (en) * | 2013-04-06 | 2013-08-07 | 西安宏冠生物科技有限公司 | Production process for extraction of chlorogenic acid from green coffee bean |
| CN103232346B (en) * | 2013-04-06 | 2016-06-08 | 西安宏冠生物科技有限公司 | A kind of production technology of green coffee bean chlorogenic acid extracting |
| CN105960171A (en) * | 2014-06-13 | 2016-09-21 | 帕万·库马·戈埃尔 | Green coffee bean extract and method thereof |
| JP2017533230A (en) * | 2014-11-26 | 2017-11-09 | スーチョアン チウチャン バイオロジカル サイエンス アンド テクノロジー カンパニー リミテッド | Method for preparing medicinal chlorogenic acid |
| CN107501094A (en) * | 2017-07-26 | 2017-12-22 | 天津泽达天健科技有限公司 | A kind of preparation method of high-purity chlorogenic acid |
| CN107879937A (en) * | 2017-10-24 | 2018-04-06 | 四川九章生物科技有限公司 | A kind of new crystal of chlorogenic acid and preparation method thereof |
| CN114478247A (en) * | 2022-03-01 | 2022-05-13 | 贵州两山康瑞食品检测科技有限公司 | Method for extracting, separating and purifying chlorogenic acid of acer truncatum leaves |
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