CN1398845A - Macroporous resin adsorption process of extracting chlorogenic acid in high content - Google Patents
Macroporous resin adsorption process of extracting chlorogenic acid in high content Download PDFInfo
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- CN1398845A CN1398845A CN 02133448 CN02133448A CN1398845A CN 1398845 A CN1398845 A CN 1398845A CN 02133448 CN02133448 CN 02133448 CN 02133448 A CN02133448 A CN 02133448A CN 1398845 A CN1398845 A CN 1398845A
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- chlorogenic acid
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Abstract
A chlorogenic acid extraction process of the present invention includes crushing honeysuckle, water extraction of chlorogenic acid and macroporous resin adsorption to separate high content chlorogenic acid. It features that in the last technological step, the chlorogenic acid extracting liquid is saturated and adsorbed with macroporous resin, the chlorogenic acid in resin is washed and dissolved with low concentration alcohol to obtain chlorogenic acid eluting liquid, the eluting liquid is concentrated while recovering alcohol and the concentrated chlorogenic acid condensate is spray-dried to obtain chlorogenic acid powder product with chlorogenic acid content over 40%. The isochlorogenic acid in the resin column is produced into powder product through methanol washing and dissolving, concentrating and spray drying, after recovering method.
Description
Technical field
The present invention relates to a kind of from Japanese Honeysuckle the processing method of chlorogenic acid extracting, particularly relate to a kind of processing method of extraction chlorogenic acid in high content with low cost.
Background technology
Chlorogenic acid is the effective constituent that mainly contains that has anti-microbial effect in the Japanese Honeysuckle.Its structure is the fat of a part coffic acid and molecule quininic acid be combined into.It is shaped as needle crystal, presents than strongly-acid, and hydrophilic solvent such as water-soluble, methyl alcohol, ethanol contains the fat key in the molecular structure, easily be hydrolyzed at alkaline environment.The extraction of chlorogenic acid, separation are the character of utilizing chlorogenic acid polarity bigger.Suitability for industrialized production adopts water cooking and extraction method, poach alcohol deposition method, 70% ethanol reflux extraction, water to carry lime precipitation chlorogenic acid extracting from Japanese Honeysuckle usually at present.All there is the low general character of product chlorogenic acid content in these methods, generally between 20%-25%; Adopt lime precipitation, the alkalescence of its lime is decomposed very big to chlorogenic acid, and the extraction method extraction cost that employing ethanol is made solvent is very high.Along with modernization of Chinese medicine process ground is accelerated, pharmacy producer requires more and more higher to Flos Lonicerae extract, and particularly American-European countries's pharmacy corporation requires the monomer composition in the Chinese medical extract pure more good more, so that qualitative and quantitative analysis, use.Up to the present, Shang Weijian has high-load chlorogenic acid launch.For adapting to the needs of the back Flos Lonicerae extract outlet of joining WTO, improve chlorogenic acid content, reducing the extraction separation cost, studying new chlorogenic acid in high content extraction and separation method is the task of top priority.
Summary of the invention
The objective of the invention is to: a kind of novel method of extracting chlorogenic acid in high content from Japanese Honeysuckle of low production cost is provided, and promptly macroporous resin adsorption is extracted the processing method of chlorogenic acid in high content.
Purpose of the present invention realizes by implementing following technical proposals:
Macroporous resin adsorption is extracted the processing method of chlorogenic acid in high content, in regular turn by the Japanese Honeysuckle raw material pulverizing, contain the aqueous extract of chlorogenic acid extraction, and the separating technology of macroporous resin adsorption chlorogenic acid in high content finished product formed; Wherein Japanese Honeysuckle raw material pulverizing technology is meant with pulverizer honeysuckle powder to be broken into the suitable particulate technology of being convenient to poach; The extraction process that contains the extracting solution of chlorogenic acid, in regular turn the soup by the Japanese Honeysuckle particle boiling operation after pulverizing, after decocting through behind the sedimentation and filtration again with vaporizer carry out spissated operation, with spissated soup add filtration operation behind the ethanol sedimentation, and filtering liquid medicine in the ethanol recovery process and will reclaim ethanol after soup carry out spissated operation and formed; The extraction process of macroporous resin adsorption chlorogenic acid in high content finished product, it is characterized in that: the condensed water extracting solution that contains chlorogenic acid that will in last technology, obtain, add in the macroporous resin column and carry out saturated absorption, chlorogenic acid and isochlorogenic acid have been stayed in the resin column after the washing, use the washing with alcohol resin column of lower concentration again, make the chlorogenic acid in the resin be obtained the chlorogenic acid elutriant by dissolve with ethanol, use high concentration methanol washing resin post again, make that isochlorogenic acid is obtained the isochlorogenic acid elutriant by dissolve with methanol in the resin; Carry out ethanol and reclaim containing alcoholic acid chlorogenic acid elutriant, the chlorogenic acid elutriant of sloughing behind the ethanol is concentrated again, then it being carried out spraying drying, promptly to obtain chlorogenic acid content be 40% finished product dry powder; The isochlorogenic acid elutriant that obtains is carried out Methanol Recovery, again the isochlorogenic acid elutriant of sloughing behind the methyl alcohol is concentrated, then its spraying drying is promptly obtained the dry powder finished product of isochlorogenic acid; The product higher as need purity, chlorogenic acid elutriant after then can be again ethanol being reclaimed as above method carries out macroporous resin column absorption and ethanol separates again, reclaim ethanol, no ethanol chlorogenic acid elutriant concentrated after again spraying drying can get the chlorogenic acid dry powder finished product of 80% content.
The invention has the advantages that: compare with existing chlorogenic acid extraction process, no matter be that water-boiling method, rare alcohol extracting are followed the example of, the poach alcohol deposition method, and water carry lime precipitation, the chlorogenic acid content of its product is low, the highlyest is no more than 25%; And technology of the present invention is brought up to 40%-80% with the chlorogenic acid content in the Flos Lonicerae extract, has both improved bacteriostasis, has reduced dosage again, and making with it is that the medicine qualitative, quantitative of raw material is more accurate.Chlorogenic acid in high content has been expanded the purposes of Japanese Honeysuckle, for products export is laid a good foundation; Not only improve flower-grower's income, and improved the economic benefit of processing enterprise; This technology reduces unit cost relatively, and added value of product increases substantially; The Flos Lonicerae extract of chlorogenic acid content 25%, about 100 yuan of current selling price per kilograms, 4 yuan of each percentage points, and the Flos Lonicerae extract of chlorogenic acid content 40%, price can reach about 600 yuan of per kilograms, each percentage point can reach 15 yuan, and the product price per kilogram of 80% above content can reach 5000 yuan, and benefit is more considerable; The present invention provides reliable material technological foundation for foreign exchange earning; Also have remarkable advantages such as technology is simple, easy to operate in addition.
Description of drawings Fig. 1 is a mark among the prior art chlorogenic acid extraction process schema figure for chlorogenic acid in high content extraction process schema Fig. 2 of the present invention: 1 is water-boiling method technology, 2 follow the example of technology for rare alcohol extracting, 3 is poach alcohol precipitator method technologies, and 4 put forward lime precipitation technology for water.
Embodiment
Macroporous resin adsorption is extracted the technology of chlorogenic acid in high content, in regular turn by the Japanese Honeysuckle raw material pulverizing, contain the aqueous extract of chlorogenic acid extraction process, and the separating technology of macroporous resin adsorption chlorogenic acid in high content finished product formed; Japanese Honeysuckle raw material pulverizing technology wherein is for the sieve pulverizer with aperture 4mm is broken into the Japanese Honeysuckle particle of particle diameter less than 4mm with honeysuckle powder; The extraction process of aqueous extract that contains chlorogenic acid is as follows: with Japanese Honeysuckle particle boiling three times.The weight ratio of Japanese Honeysuckle and water is 1: 5 for the first time, decocts taking liquid 2 hours; Weight ratio with boiling for the third time is 1: 3 for the second time, decocted respectively 30 minutes, the soup of three decoctions is merged, precipitate and get supernatant liquid filtering after 20 hours, then filtered liquid is concentrated into the clear cream of certain density with thin-film evaporator or external circulation evaporator, be chilled to about 40 ℃, under agitation slowly add a certain amount of ethanol, only put 24 hours, get supernatant liquid filtering, making ethanol reclaim filtrate with distillation method filtrate does not then have the alcohol flavor, adds certain water gaging and activated carbon then, little boiling 10 minutes, filtered while hot leaves standstill after 12 hours filtrate and gets supernatant liquid filtering, and the ratio that is concentrated into medicine and water is 3: 1 a clear cream, put the aqueous extract that just becomes to contain chlorogenic acid after cold, more than filter and all adopt tubular-bowl centrifuge to separate to carry out; Macroporous resin adsorption chlorogenic acid in high content finished product extraction process is as follows: the resin column of strongly basic anion macroporous resin will be housed, wash with methyl alcohol earlier, and clean with clear water; The aqueous extract that will contain chlorogenic acid adds in the resin column saturated to resin, it is colourless to effluent liquid to wash resin column with water, stay chlorogenic acid and isochlorogenic acid this moment in the resin column, use the ethanol that hangs down the number of degrees generally to use the ethanol of 5-15% again, best ethanol elution with 10% does not have chlorogenic acid to making in the resin column, stay the resin that contains isochlorogenic acid, use the methyl alcohol of the higher number of degrees again, general methyl alcohol with 30-50%, best methanol-eluted fractions resin column to effluent liquid with 40% does not contain isochlorogenic acid, eluted resin post then carries out after the manipulation of regeneration resin stand-by; The elutriant that contains chlorogenic acid and ethanol and isochlorogenic acid and methyl alcohol respectively that aforementioned wash-out is come out, carry out the recycling of ethanol and methyl alcohol respectively, to remove again behind ethanol and the methyl alcohol two kinds of elutriants respectively concentrating under reduced pressure become thick paste, spraying drying promptly obtains the chlorogenic acid and the isochlorogenic acid dry powder of 40% above content.Carry out single step purification as need, the chlorogenic acid elutriant after ethanol is reclaimed, fractionation by adsorption more as stated above is just can obtain the chlorogenic acid dry powder of 80% above content.
Claims (3)
1, macroporous resin adsorption is extracted the processing method of chlorogenic acid in high content, in regular turn by the Japanese Honeysuckle raw material pulverizing, contain the aqueous extract of chlorogenic acid extraction, and the separating technology of macroporous resin adsorption chlorogenic acid in high content finished product formed; Wherein Japanese Honeysuckle raw material pulverizing technology is meant with pulverizer honeysuckle powder to be broken into the suitable particulate technology of being convenient to poach; The extraction process that contains the extracting solution of chlorogenic acid, in regular turn the soup by the Japanese Honeysuckle particle boiling operation after pulverizing, after decocting through behind the sedimentation and filtration again with vaporizer carry out spissated operation, with spissated soup add filtration operation behind the ethanol sedimentation, and filtering liquid medicine in the ethanol recovery process and will reclaim ethanol after soup carry out spissated operation and formed; The extraction process of macroporous resin adsorption chlorogenic acid in high content finished product, it is characterized in that: the condensed water extracting solution that contains chlorogenic acid that will in last technology, obtain, add in the macroporous resin column and carry out saturated absorption, chlorogenic acid and isochlorogenic acid have been stayed in the resin column after the washing, use the washing with alcohol resin column of lower concentration again, make the chlorogenic acid in the resin be obtained the chlorogenic acid elutriant by dissolve with ethanol, use high concentration methanol washing resin post again, make that isochlorogenic acid is obtained the isochlorogenic acid elutriant by dissolve with methanol in the resin; Carry out ethanol and reclaim containing alcoholic acid chlorogenic acid elutriant, the chlorogenic acid elutriant of sloughing behind the ethanol is concentrated again, then it being carried out spraying drying, promptly to obtain chlorogenic acid content be 40% finished product dry powder; The isochlorogenic acid elutriant that obtains is carried out Methanol Recovery, again the isochlorogenic acid elutriant of sloughing behind the methyl alcohol is concentrated, then its spraying drying is promptly obtained the dry powder finished product of isochlorogenic acid; The product higher as need purity, chlorogenic acid elutriant after then can be again ethanol being reclaimed as above method carries out macroporous resin column absorption and ethanol separates again, reclaim ethanol, no ethanol chlorogenic acid elutriant concentrated after again spraying drying can get the chlorogenic acid dry powder finished product of 80% content.
2, extract the processing method of chlorogenic acid in high content according to the described macroporous resin adsorption of claim 1, it is characterized in that: the condensed water extracting solution that will contain chlorogenic acid adds in the macroporous resin column and carries out saturated absorption, chlorogenic acid and isochlorogenic acid have been stayed in the resin column after the washing, be the washing with alcohol resin column of 5-15% with concentration again, make the chlorogenic acid in the resin be obtained the chlorogenic acid elutriant by dissolve with ethanol; Be the methanol wash resin column of 30-50% with concentration again, make that isochlorogenic acid is obtained the isochlorogenic acid elutriant by dissolve with methanol in the resin.
3, extract the processing method of chlorogenic acid in high content according to the described macroporous resin adsorption of claim 2, it is characterized in that: be used for washing dissolving resin post chlorogenic acid, the ethanol optimum concn of chlorogenic acid extracting elutriant is 10%, be used for washing dissolving resin post isochlorogenic acid, the methyl alcohol optimum concn of extracting the isochlorogenic acid elutriant is 40%.
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006241006A (en) * | 2005-03-01 | 2006-09-14 | Kao Corp | Method for producing chlorogenic acid composition |
| CN101933967A (en) * | 2010-08-31 | 2011-01-05 | 蚌埠丰原涂山制药有限公司 | Honeysuckle extract preparation method |
| CN101314568B (en) * | 2008-06-24 | 2011-05-11 | 南京工业大学 | Novel method for adsorbing and separating high-purity chlorogenic acid |
| 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 |
| CN103823034A (en) * | 2014-03-06 | 2014-05-28 | 山东省食品药品检验所 | Honeysuckle contrasting extract and preparation method thereof |
| CN104399280A (en) * | 2014-11-26 | 2015-03-11 | 四川九章生物科技有限公司 | Device for enriching and purifying compounds and use method of device |
| CN105394808A (en) * | 2015-12-17 | 2016-03-16 | 立场电子科技发展（上海）有限公司 | Atomization liquid for electronic cigarette |
| CN107375393A (en) * | 2017-07-14 | 2017-11-24 | 临沂大学 | A kind of honeysuckle organic acid constituents coating of pellets particle and preparation method thereof |
| CN107602385A (en) * | 2017-08-18 | 2018-01-19 | 合肥丰洁生物科技有限公司 | A kind of process of the chlorogenic acid extracting from honeysuckle |
| CN110898095A (en) * | 2018-09-17 | 2020-03-24 | 泰州医药城国科化物生物医药科技有限公司 | Honeysuckle refined product and preparation method and application thereof |
| CN114957020A (en) * | 2022-06-10 | 2022-08-30 | 贵州两山康瑞食品检测科技有限公司 | Method for extracting and purifying choline from acer truncatum leaves |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101837039B (en) * | 2009-03-20 | 2012-01-25 | 上海中医药大学 | Chlorogenic acid-free honeysuckle extract and preparation method |
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2002
- 2002-07-10 CN CNB02133448XA patent/CN1168698C/en not_active Expired - Fee Related
Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101133015B (en) * | 2005-03-01 | 2010-06-16 | 花王株式会社 | Method of producing chlorogenic acid composition |
| US8309150B2 (en) | 2005-03-01 | 2012-11-13 | Kao Corporation | Method of producing chlorogenic acid composition |
| JP2006241006A (en) * | 2005-03-01 | 2006-09-14 | Kao Corp | Method for producing chlorogenic acid composition |
| CN101314568B (en) * | 2008-06-24 | 2011-05-11 | 南京工业大学 | Novel method for adsorbing and separating high-purity chlorogenic acid |
| CN101933967A (en) * | 2010-08-31 | 2011-01-05 | 蚌埠丰原涂山制药有限公司 | Honeysuckle extract preparation method |
| CN101933967B (en) * | 2010-08-31 | 2012-06-13 | 蚌埠丰原涂山制药有限公司 | Honeysuckle extract preparation method |
| 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 |
| 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 |
| CN103823034A (en) * | 2014-03-06 | 2014-05-28 | 山东省食品药品检验所 | Honeysuckle contrasting extract and preparation method thereof |
| CN103823034B (en) * | 2014-03-06 | 2016-03-09 | 山东省食品药品检验研究院 | A kind of honeysuckle reference extract and preparation method thereof |
| CN104399280A (en) * | 2014-11-26 | 2015-03-11 | 四川九章生物科技有限公司 | Device for enriching and purifying compounds and use method of device |
| CN105394808A (en) * | 2015-12-17 | 2016-03-16 | 立场电子科技发展（上海）有限公司 | Atomization liquid for electronic cigarette |
| CN107375393A (en) * | 2017-07-14 | 2017-11-24 | 临沂大学 | A kind of honeysuckle organic acid constituents coating of pellets particle and preparation method thereof |
| CN107375393B (en) * | 2017-07-14 | 2021-05-07 | 临沂大学 | Honeysuckle organic acid component pellet coating granule and preparation method thereof |
| CN107602385A (en) * | 2017-08-18 | 2018-01-19 | 合肥丰洁生物科技有限公司 | A kind of process of the chlorogenic acid extracting from honeysuckle |
| CN110898095A (en) * | 2018-09-17 | 2020-03-24 | 泰州医药城国科化物生物医药科技有限公司 | Honeysuckle refined product and preparation method and application thereof |
| CN114957020A (en) * | 2022-06-10 | 2022-08-30 | 贵州两山康瑞食品检测科技有限公司 | Method for extracting and purifying choline from acer truncatum leaves |
| CN114957020B (en) * | 2022-06-10 | 2024-03-08 | 贵州两山康瑞食品检测科技有限公司 | Method for extracting and purifying choline from acer truncatum leaves |
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