CN1616403A - Process for preparing chlorogenic acid from honeysuckle - Google Patents
Process for preparing chlorogenic acid from honeysuckle Download PDFInfo
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- CN1616403A CN1616403A CN 200410035758 CN200410035758A CN1616403A CN 1616403 A CN1616403 A CN 1616403A CN 200410035758 CN200410035758 CN 200410035758 CN 200410035758 A CN200410035758 A CN 200410035758A CN 1616403 A CN1616403 A CN 1616403A
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- japanese honeysuckle
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Abstract
The present invention relates to process of extracting chlorogenic acid from honeysuckle and belongs to the field of medicinal chemical technology. The process includes the steps of: reflux extraction of honeysuckle with water or ethanol, filtering to collect filtrate, recovering solvent, ethanol deposition to eliminating impurity, letting stand overnight, filtering, decompression recovering solvent, adding water and letting stand overnight, filtering, eluting the filtrate in macroporous resin column, concentrating eluent, collecting chlorogenic acid component, eluting on polyamide column with eluent, collecting chlorogenic acid component, concentration, rectification to obtain chlorogenic acid product with content over 95 %. The present invention is suitable for industrial application.
Description
Technical field
The present invention relates to a kind of from Japanese Honeysuckle the processing method of extraction separation chlorogenic acid.
Background technology
Japanese Honeysuckle is a kind of conventional Chinese medicine, and long medicinal history is arranged.Traditional medicine thinks that Japanese Honeysuckle has function clearing heat and detoxicating, wind-heat dissipating, clinically diseases such as warm disease heating, common cold due to wind-heat, swelling and pain in the throat, pneumonia, erysipelas that are used for the treatment of more.Middle regulation chlorogenic acid of Pharmacopoeia of the People's Republic of China version in 2000 is the index components in the Japanese Honeysuckle, and its content must not be less than 1.5%.But chlorogenic acid content is extremely unstable in the Japanese Honeysuckle, is subject to the influence of multiple internal and external factor and changes.Medical research and facts have proved that chlorogenic acid is a most important activeconstituents in the Japanese Honeysuckle.Chlorogenic acid has anti-microbial effect widely, cholagogic is arranged, stop blooding, increase white cell and antivirus action, has the blood clotting of shortening and the effect in bleeding time.Clinical application is in treating upper respiratory tract infection, anti inflammation and heat resolution, cool blood heat radiation.
The traditional technology of at present chlorogenic acid in the Japanese Honeysuckle being extracted has water-boiling method, water extract-alcohol precipitation, extraction, macroporous resin adsorption etc.But because the unstable characteristic of chlorogenic acid, in the extraction separation process, usually be accompanied by the decomposition of chlorogenic acid, be difficult to make content to reach more than 90%, as the extracting method put down in writing in the Chinese patent 01144170.4 can only dna purity reach 84%, the extracting method put down in writing among the Chinese patent 02133448.X can only reach 80% by dna purity.Though some breadboard preparation method can obtain higher purity, can't carry out large-scale industrial production.Therefore, though the determined curative effect of chlorogenic acid can't be declared first class national new drug owing to the technical reason of extraction separation always.
Summary of the invention
The invention reside in provides a kind of technology of extracting the preparation chlorogenic acid from Japanese Honeysuckle, from Japanese Honeysuckle through extracting content greater than 95% chlorogenic acid monomer.
Technical scheme of the present invention is: this kind extracts the technology of preparation chlorogenic acid from Japanese Honeysuckle, it is characterized in that Japanese Honeysuckle adds water or ethanol carries out refluxing extraction, filter, collect filtrate and reclaim solvent, add ethanol sedimentation impurity, spend the night, filter, decompression and solvent recovery, it is an amount of to add water, standing over night, filter, macroporous resin column on the filtrate concentrates with eluent, collection contains the component of chlorogenic acid, last polyamide column is used the eluent wash-out, collects the component that contains chlorogenic acid, concentrate, the refining content that obtains is greater than 95% chlorogenic acid.
In the preceding method, concentration of ethanol is 0～80% during extraction, preferably 30-70%.Also can only use water extraction.
In the preceding method, described macroporous resin is to meet medicinal requirements, and granularity is 20～60 purpose styrene type resins or vinyl cyanide type resin.Refer in particular to DM130 and D101 type macroporous resin.
In the preceding method, described eluent is a water, also can use ethanol.
In the preceding method, described process for purification is an organic solvent extraction, and wherein organic solvent refers to ethyl acetate or primary isoamyl alcohol; Described process for purification also can be used the silica gel chromatography column purification.
In the preceding method, refluxing extraction three times, each time is 2.5-3.5 hour, Japanese Honeysuckle is 1: 5 with the ratio of water or ethanol.
Other detail are common in this area.
The extraction separation of chlorogenic acid of the present invention comprises following concrete steps:
1). Japanese Honeysuckle is packed in the extractor, add the solvent of 5 times of weight of relative Japanese Honeysuckle, extract three times by extracting the temperature heating usually, each time 2.5-3.5 hour, filter, reclaim solvent, add ethanol and make contamination precipitation; Standing over night.
2). filter, discard precipitation, filtrate is concentrated into no ethanol, and it is an amount of to add water, standing over night.
3). filter, the good macroporous resin column of pre-treatment on the filtrate, water and ethanol elution are collected the component that contains chlorogenic acid, polyamide column in the merging, water and ethanol elution are collected the component that contains chlorogenic acid, merge.
4). the elutriant that will contain chlorogenic acid is concentrated into every milliliter and contains the 2g raw medicinal herbs, with primary isoamyl alcohol or ethyl acetate extraction; Reclaim solvent and drying and obtain the chlorogenic acid elaboration.
5). above-mentioned steps 4 also can concentrate the elutriant of chlorogenic acid, drying under reduced pressure.Dry thing is gone up preparation type silica gel chromatographic column again, and wash-out is after conventional processing obtains the chlorogenic acid elaboration.
6). the chlorogenic acid elaboration of gained, handle through corresponding preparations, add N.F,USP MANNITOL, obtain the powder pin of chlorogenic acid through the freeze-drying can.
The invention has the beneficial effects as follows: present method can industrialization ground from Japanese Honeysuckle, obtain content greater than 95% chlorogenic acid monomer, and extraction cost and not obvious raising.This provides the industrialization guarantee for a large amount of powder pins that obtain chlorogenic acid.
Embodiment
Embodiment one:
The 500g Japanese Honeysuckle is packed in the extractor, adds the water of 5 times of weight of Japanese Honeysuckle, and heating is extracted three times, and each time is 3.5 hours.The medical filtration decompression and solvent recovery adds medicinal ethanol sedimentation, makes to contain alcohol amount at last and reach 75%, standing over night, filter or centrifugal, discard precipitation, filtrate is concentrated into no ethanol, adds water and makes every milliliter to contain 2g crude drug amount be 0.5g, standing over night is filtered or the centrifugal precipitation that discards macroporous resin column on the filtrate.Water and 10% ethanol elution utilize the thin-layer chromatography inspection, collect the component that contains chlorogenic acid, last polyamide column, water and 10% ethanol elution are collected the component that contains chlorogenic acid, the elutriant that will contain chlorogenic acid is concentrated into every milliliter and contains the 2g crude drug, extracts with primary isoamyl alcohol.Reclaim solvent, obtain enriched material, drying gets chlorogenic acid elaboration 8g, and content is greater than 95%.
Embodiment two:
The 250g Japanese Honeysuckle is packed in the extractor, adds the ethanol of 5 times of crude drug weight, heating and refluxing extraction three times, time is 3 hours, filters, and filtrate is reclaimed solvent, add water and make every milliliter to contain crude drug amount 0.5g, standing over night is filtered or the centrifugal precipitation that discards, macroporous resin column on the filtrate, water and 10% ethanol elution are collected the component that contains chlorogenic acid, last polyamide column, water and 10% ethanol elution are collected the component that contains chlorogenic acid, be concentrated into every milliliter and contain the 2g crude drug, extract with ethyl acetate.Reclaim solvent, obtain enriched material, drying gets content greater than 95% chlorogenic acid elaboration 4g.
Embodiment three:
The 1250g Japanese Honeysuckle is packed into and adds 30% ethanol of 5 times of amounts in the extractor, heating is extracted three times, and the time is 2.5 hours, filters, filtrate is reclaimed solvent, add medicinal ethanol and make the alcohol amount 50% that contains, standing over night is filtered or the centrifugal precipitation that discards, macroporous resin column on the filtrate, water and 10% ethanol elution are collected the component that contains chlorogenic acid, last polyamide column, water and 10% ethanol elution, collection contains the component of chlorogenic acid, is concentrated into the medicinal extract shape, drying under reduced pressure, last silica gel chromatographic column, use the ethyl acetate-ethanol wash-out, reclaim eluent, obtain content greater than 98% chlorogenic acid crystal.
Embodiment four:
Get chlorogenic acid elaboration 15g, be dissolved in water for injection, add N.F,USP MANNITOL 45g, lyophilize obtains chlorogenic acid powder pin.
Claims (7)
1, a kind of technology of from Japanese Honeysuckle, extracting the preparation chlorogenic acid, it is characterized in that: Japanese Honeysuckle adds water/ethanol and carries out refluxing extraction, filters, and collects filtrate and reclaims solvent, add ethanol sedimentation impurity, spend the night, filter, decompression and solvent recovery, it is an amount of to add water, standing over night, filter, macroporous resin column on the filtrate concentrates with eluent, collection contains the component of chlorogenic acid, and last polyamide column is used the eluent wash-out, collection contains the component of chlorogenic acid, concentrates, and the refining content that obtains is greater than 95% chlorogenic acid.
2, the technology of extracting the preparation chlorogenic acid from Japanese Honeysuckle according to claim 1, concentration of ethanol is 0～80% when it is characterized in that extracting.
3, the technology of extracting the preparation chlorogenic acid from Japanese Honeysuckle according to claim 1 and 2 is characterized in that described macroporous resin is to meet medicinal requirements, and granularity is 20～60 purpose styrene type resins or vinyl cyanide type resin.
4, the technology of extracting the preparation chlorogenic acid from Japanese Honeysuckle according to claim 3 is characterized in that described styrene type resin or vinyl cyanide type resin, refers in particular to DM130 and D101 type macroporous resin.
5, the technology of extracting the preparation chlorogenic acid from Japanese Honeysuckle according to claim 1 is characterized in that described eluent is water and ethanol.
6, the technology of extracting the preparation chlorogenic acid from Japanese Honeysuckle according to claim 1 is characterized in that described process for purification is organic solvent extraction or silica gel chromatography column purification, and wherein organic solvent refers to ethyl acetate or primary isoamyl alcohol.
7, the technology of extracting the preparation chlorogenic acid from Japanese Honeysuckle according to claim 1 is characterized in that refluxing extraction three times, and each time is 2.5-3.5 hour, and Japanese Honeysuckle is 1: 5 with the ratio of water or ethanol.
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200410035758 CN1616403A (en) | 2004-09-21 | 2004-09-21 | Process for preparing chlorogenic acid from honeysuckle |
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| CN 200410035758 CN1616403A (en) | 2004-09-21 | 2004-09-21 | Process for preparing chlorogenic acid from honeysuckle |
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Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100338017C (en) * | 2005-09-29 | 2007-09-19 | 深圳清华大学研究院 | Method for preparing high-purity chlorogenic acid from honeysuckle crude extract |
| CN100341845C (en) * | 2005-09-10 | 2007-10-10 | 江南大学 | Chlorogenic acid extracting and purifying process from sunflower seed dregs |
| US7314644B2 (en) * | 2002-09-11 | 2008-01-01 | Sk Chemicals Co., Ltd. | Extraction and purification method of active constituents from stem of Lonicera japonica thunb., its usage for anti-inflammatory and analgesic drug |
| CN101823964A (en) * | 2010-03-12 | 2010-09-08 | 山东大学威海分校 | Technology for preparing chlorogenic acid in viburnum sargentii koehne leaves |
| CN101250106B (en) * | 2008-03-27 | 2011-05-18 | 北京市农林科学院 | Method for extracting chlorogenic acid |
| CN101837039B (en) * | 2009-03-20 | 2012-01-25 | 上海中医药大学 | Chlorogenic acid-free honeysuckle extract and preparation method |
| CN102552369A (en) * | 2012-02-14 | 2012-07-11 | 陈剑锋 | Lon icera japonica Thunb leaf extractive serving as anti-porcine reproductive and respiratory syndrome viral agent |
| CN102942483A (en) * | 2012-10-19 | 2013-02-27 | 湖北楚天舒药业有限公司 | Method for preparing a plurality of caffeoylquinic acid monomers from honeysuckle |
| 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 |
| CN103446064A (en) * | 2013-08-21 | 2013-12-18 | 四川九章生物化工科技发展有限公司 | Chlorogenic acid powder-injection and preparation method thereof |
| CN103787885A (en) * | 2014-03-06 | 2014-05-14 | 山东禾本堂生物科技有限公司 | Method of extracting chlorogenic acid with high purity from honeysuckle above ground part |
| CN104086424A (en) * | 2014-07-11 | 2014-10-08 | 广州中大南沙科技创新产业园有限公司 | Method for extracting and separating chlorogenic acid from honeysuckle flower |
| CN104130127A (en) * | 2014-06-18 | 2014-11-05 | 广西万寿堂药业有限公司 | Process method for extracting chlorogenic acid from blumea riparia(BL.)DC |
| WO2015024217A1 (en) * | 2013-08-21 | 2015-02-26 | 四川九章生物科技有限公司 | Chlorogenic acid powder-injection and preparation method thereof |
| CN105367424A (en) * | 2015-12-24 | 2016-03-02 | 攀枝花市西宇生物科技有限公司 | Method for preparing high-purity chlorogenic acid from eupatorium adenophorum Spreng |
| CN106008212A (en) * | 2016-06-14 | 2016-10-12 | 江苏天晟药业股份有限公司 | Preparing method for chlorogenic acid and similar compounds thereof |
| CN106259833A (en) * | 2016-08-18 | 2017-01-04 | 华南理工大学 | Improve the Flos Lonicerae extract of cold preservation pork product quality and preparation method thereof and purposes |
| CN107007674A (en) * | 2017-04-17 | 2017-08-04 | 四川阿尔康生物工程有限责任公司 | A kind of clearing lung-heat soft capsule and preparation method thereof |
| CN108771066A (en) * | 2018-05-21 | 2018-11-09 | 遵义市郎笑笑食品有限责任公司 | A kind of honeysuckle beverage processing technology |
-
2004
- 2004-09-21 CN CN 200410035758 patent/CN1616403A/en active Pending
Cited By (26)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7314644B2 (en) * | 2002-09-11 | 2008-01-01 | Sk Chemicals Co., Ltd. | Extraction and purification method of active constituents from stem of Lonicera japonica thunb., its usage for anti-inflammatory and analgesic drug |
| CN100341845C (en) * | 2005-09-10 | 2007-10-10 | 江南大学 | Chlorogenic acid extracting and purifying process from sunflower seed dregs |
| CN100338017C (en) * | 2005-09-29 | 2007-09-19 | 深圳清华大学研究院 | Method for preparing high-purity chlorogenic acid from honeysuckle crude extract |
| CN101250106B (en) * | 2008-03-27 | 2011-05-18 | 北京市农林科学院 | Method for extracting chlorogenic acid |
| CN101837039B (en) * | 2009-03-20 | 2012-01-25 | 上海中医药大学 | Chlorogenic acid-free honeysuckle extract and preparation method |
| CN101823964A (en) * | 2010-03-12 | 2010-09-08 | 山东大学威海分校 | Technology for preparing chlorogenic acid in viburnum sargentii koehne leaves |
| CN102552369A (en) * | 2012-02-14 | 2012-07-11 | 陈剑锋 | Lon icera japonica Thunb leaf extractive serving as anti-porcine reproductive and respiratory syndrome viral agent |
| CN102942483A (en) * | 2012-10-19 | 2013-02-27 | 湖北楚天舒药业有限公司 | Method for preparing a plurality of caffeoylquinic acid monomers from honeysuckle |
| 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 |
| CN103446064A (en) * | 2013-08-21 | 2013-12-18 | 四川九章生物化工科技发展有限公司 | Chlorogenic acid powder-injection and preparation method thereof |
| US9918956B2 (en) | 2013-08-21 | 2018-03-20 | Sichuan Jiuzhang Biological Science And Technology Co., Ltd | Chlorogenic acid powder-injection and preparation method thereof |
| WO2015024217A1 (en) * | 2013-08-21 | 2015-02-26 | 四川九章生物科技有限公司 | Chlorogenic acid powder-injection and preparation method thereof |
| CN103446064B (en) * | 2013-08-21 | 2015-04-15 | 四川九章生物科技有限公司 | Chlorogenic acid powder-injection and preparation method thereof |
| EP3040067A4 (en) * | 2013-08-21 | 2017-03-22 | Sichuan Jiuzhang Biological Science And Technology Co., Ltd | Chlorogenic acid powder-injection and preparation method thereof |
| CN103787885A (en) * | 2014-03-06 | 2014-05-14 | 山东禾本堂生物科技有限公司 | Method of extracting chlorogenic acid with high purity from honeysuckle above ground part |
| CN104130127A (en) * | 2014-06-18 | 2014-11-05 | 广西万寿堂药业有限公司 | Process method for extracting chlorogenic acid from blumea riparia(BL.)DC |
| CN104130127B (en) * | 2014-06-18 | 2016-09-28 | 广西万寿堂药业有限公司 | A kind of process extracting chlorogenic acid from Herba Blumeae Balsamiferae |
| CN104086424B (en) * | 2014-07-11 | 2016-01-27 | 广州中大南沙科技创新产业园有限公司 | A kind of method of extraction and isolation chlorogenic acid from Lonicera confusa DC. |
| CN104086424A (en) * | 2014-07-11 | 2014-10-08 | 广州中大南沙科技创新产业园有限公司 | Method for extracting and separating chlorogenic acid from honeysuckle flower |
| CN105367424A (en) * | 2015-12-24 | 2016-03-02 | 攀枝花市西宇生物科技有限公司 | Method for preparing high-purity chlorogenic acid from eupatorium adenophorum Spreng |
| CN105367424B (en) * | 2015-12-24 | 2018-06-19 | 攀枝花市西宇生物科技有限公司 | The method that high-purity chlorogenic acid is prepared with Eupatorium adenophorum |
| CN106008212A (en) * | 2016-06-14 | 2016-10-12 | 江苏天晟药业股份有限公司 | Preparing method for chlorogenic acid and similar compounds thereof |
| CN106259833A (en) * | 2016-08-18 | 2017-01-04 | 华南理工大学 | Improve the Flos Lonicerae extract of cold preservation pork product quality and preparation method thereof and purposes |
| CN107007674A (en) * | 2017-04-17 | 2017-08-04 | 四川阿尔康生物工程有限责任公司 | A kind of clearing lung-heat soft capsule and preparation method thereof |
| CN108771066A (en) * | 2018-05-21 | 2018-11-09 | 遵义市郎笑笑食品有限责任公司 | A kind of honeysuckle beverage processing technology |
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