CN101503357A - Method for extracting chlorogenic acid in honeysuckle - Google Patents
Method for extracting chlorogenic acid in honeysuckle Download PDFInfo
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- CN101503357A CN101503357A CNA2009101163842A CN200910116384A CN101503357A CN 101503357 A CN101503357 A CN 101503357A CN A2009101163842 A CNA2009101163842 A CN A2009101163842A CN 200910116384 A CN200910116384 A CN 200910116384A CN 101503357 A CN101503357 A CN 101503357A
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- honeysuckle
- chlorogenic acid
- japanese honeysuckle
- ethyl acetate
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Abstract
The invention relates to a method for extracting chlorogenic acid in honeysuckle, belonging to the technical field of chemical engineering. The invention aims at providing the method for extracting chlorogenic acid in honeysuckle, so as to solve the problem that the existing chlorogenic acid extract is difficult to filter caused by a great amount of precipitation generated in the process of impurity removal and purification, thus improving the purity and yield of the product. Meanwhile, when the chlorogenic acid in the honeysuckle is extracted, a series of products with higher added value can be produced, so that the raw material resource of the honeysuckle can be better utilized. The method comprises the technical key points: the ground honeysuckle is leached in a dynamic state by petroleum ether, and fragrant extract of the honeysuckle in obtained by concentration after the extracting solution is filtered and the petroleum ether is recovered; after the petroleum ether is leached, the honeysuckle is extracted by reflux by using ethyl acetate, and the ethyl acetate is recovered after the extracting solution is filtered, so that honeysuckle general flavone is obtained by concentration; the honeysuckle processed by reflux extraction by using ethyl acetate is added with water for dynamic extraction, and the extracting solution is filtered, decompressed, concentrated, deposited in alcohol, decolored, purified, concentrated and dried, so that the chlorogenic acid in the honeysuckle can be obtained.
Description
Technical field:
The present invention relates to the extracting process of chlorogenic acid in a kind of Japanese Honeysuckle, belong to chemical technology field.
Background technology:
Japanese Honeysuckle is the caprifoliaceae plant dry flower of honeysuckle, and main effective constituent is chlorogenic acid, and soluble in water, pure and mild acetone equal solvent is insoluble to sherwood oil, is slightly soluble in ethyl acetate.At present from the method for Japanese Honeysuckle chlorogenic acid extracting mainly contain that water is carried, water extract-alcohol precipitation and rare ethanol-extracted etc., processes such as concentrating and precipitating impurity elimination are all arranged, in this process, have precipitation capacity big, filter time consumption and energy consumption and because of the precipitation disadvantages such as the chlorogenic acid loss amount is bigger of carrying under one's arms.
Summary of the invention:
The object of the present invention is to provide the extracting process of chlorogenic acid in a kind of Japanese Honeysuckle,, improve the purity and the yield of product to solve the filtration difficulty that present chlorogenic acid extract causes greatly because of precipitation capacity in the impurity elimination purge process; And when extracting Flos Lonicerae chlorogenic acid, produce a series of added value high product, the raw material resources of better utilised Japanese Honeysuckle.
Its technical scheme is: the extracting process of chlorogenic acid in a kind of Japanese Honeysuckle is characterized in that: ground honeysuckle is carried out dynamic lixiviate with sherwood oil, after extracting solution reclaims sherwood oil after filtration, concentrate and obtain gold and silver fragrance of a flower medicinal extract; Japanese Honeysuckle after the sherwood oil lixiviate carries out refluxing extraction with ethyl acetate again, and extracting solution reclaims ethyl acetate after filtering, concentrates to obtain the Japanese Honeysuckle total flavones; Japanese Honeysuckle after ethyl acetate backflow is extracted adds water, dynamic extraction, extracting solution after filtration, decompression, concentrate, alcohol precipitation, decolouring, purifying, concentrate, dry, promptly get Flos Lonicerae chlorogenic acid.
Its technique effect is: the present invention utilizes chlorogenic acid to be insoluble to sherwood oil, and wax, fat-soluble anthocyanidin, volatile oil are dissolved in the principle of sherwood oil, go out the higher byproduct of added value--gold and silver fragrance of a flower medicinal extract and Japanese Honeysuckle total flavones in the Japanese Honeysuckle, except that chlorogenic acid with sherwood oil and ethyl acetate extraction in advance, waste and loss had both been avoided to the Japanese Honeysuckle raw material resources, simultaneously also be process, reduced the filtration difficulty in chlorogenic acid water extract alcohol precipitation stage an impurity elimination purifying of chlorogenic acid extracting; In addition,, the later stage macroporous resin greatly increased to the treatment capacity of chlorogenic acid liquid, improved product purity and yield owing to extracted the major part in the Japanese Honeysuckle and the flavones and the tannin of chlorogenic acid structural similitude in advance.
Embodiment:
Embodiment 1.Get the Japanese Honeysuckle 200g after the pulverizing, with the 1000g sherwood oil 30 ℃ ± 2 ℃ dynamic extraction 6 hours, leach solution after, repeat to extract once with 1000g live oil ether again.Merge solution, get Flos Lonicerae extractum behind the recovery sherwood oil, other puts.
Japanese Honeysuckle after the sherwood oil lixiviate with the 600g ethyl acetate, was refluxed 30 minutes, leached extracting solution, repeated to extract once with the 600g ethyl acetate again.United extraction liquid after the recovery ethyl acetate, gets isabelline extract, and chemical qualitativity is mainly flavonoid compound, and other puts.
Japanese Honeysuckle after the ethyl acetate extraction adds 2000g water dynamic extraction 1 hour under 60 ℃ of conditions, filters to get filtrate; Repeat to extract once with 2000g water again.Merging filtrate, 60 ℃ are evaporated to soup than being 1:0.8, add the ethanol 800g of alcoholic strength 95%, staticly settle and filter, filtrate recycling ethanol is to there not being the alcohol flavor, behind 3% activated carbon decolorizing, with NKA-9 type macroporous resin mixing, absorption is in the NKA-9 type macroporous resin chromatography column of then it being packed into, press the washing of 5ml/min speed with deionized water, wash to the deionized water water white transparency.
With 30% ethanol, 3ml/min speed wash-out and dehydrate the chlorogenic acid crude product.Conversion rate of products is 85%, and chlorogenic acid content is 43.3% (high performance liquid phase).
Embodiment 2.Get the Japanese Honeysuckle 300g after the pulverizing, with the 1500g sherwood oil 30 ℃ ± 2 ℃ dynamic extraction 8 hours, leach solution after, repeat to extract once with 1500g live oil ether again.Merge solution, get Flos Lonicerae extractum behind the recovery sherwood oil, other puts.
Japanese Honeysuckle after the sherwood oil lixiviate with the 900g ethyl acetate, was refluxed 30 minutes, leached extracting solution, repeated to extract once with the 900g ethyl acetate again.United extraction liquid after the recovery ethyl acetate, gets isabelline extract, and chemical qualitativity is mainly flavonoid compound, and other puts.
Japanese Honeysuckle after the ethyl acetate extraction adds 3000g water dynamic extraction 1 hour under 60 ℃ of conditions, filters to get filtrate; Repeat to extract once with 2000g water again.Merging filtrate, 60 ℃ are evaporated to soup than being 1:0.9, add the ethanol 900ml of alcoholic strength 90%, staticly settle and filter, and filtrate recycling ethanol behind 3% activated carbon decolorizing, adopts supermembrane to filter purifying to there not being the alcohol flavor.With 30% ethanol, 3ml/min speed wash-out and dehydrate the chlorogenic acid crude product.The conversion rate of products 85% of technical process, chlorogenic acid content 43.3% (high performance liquid phase).
Claims (6)
1, the extracting process of chlorogenic acid in a kind of Japanese Honeysuckle is characterized in that: ground honeysuckle is carried out dynamic lixiviate with sherwood oil, after extracting solution reclaims sherwood oil after filtration, concentrate and obtain gold and silver fragrance of a flower medicinal extract; Japanese Honeysuckle after the sherwood oil lixiviate carries out refluxing extraction with ethyl acetate again, and extracting solution reclaims ethyl acetate after filtering, concentrates to obtain the Japanese Honeysuckle total flavones; Japanese Honeysuckle after ethyl acetate backflow is extracted adds water, dynamic extraction, extracting solution after filtration, decompression, concentrate, alcohol precipitation, decolouring, purifying, concentrate, dry, promptly get Flos Lonicerae chlorogenic acid.
2, the extracting process of chlorogenic acid in the Japanese Honeysuckle according to claim 1, it is characterized in that: the mass ratio of sherwood oil and Japanese Honeysuckle is 5:1, under the normal temperature state, dynamic soaking 6-8 hours.
3, the extracting process of chlorogenic acid in the Japanese Honeysuckle according to claim 1 and 2 is characterized in that: with sherwood oil Japanese Honeysuckle is carried out dynamic lixiviate secondary.
4, the extracting process of chlorogenic acid in the Japanese Honeysuckle according to claim 1, it is characterized in that: the mass ratio of ethyl acetate and Japanese Honeysuckle is 3:1.
5, according to the extracting process of chlorogenic acid in claim 1 or the 4 described Japanese Honeysuckles, it is characterized in that: the Japanese Honeysuckle after the sherwood oil lixiviate, extract secondary with ethyl acetate backflow.
6, the extracting process of chlorogenic acid in the Japanese Honeysuckle according to claim 1 is characterized in that: purifying process adopts macroporous resin adsorption, impurity elimination purifying or filter purifying with supermembrane.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2009101163842A CN101503357A (en) | 2009-03-20 | 2009-03-20 | Method for extracting chlorogenic acid in honeysuckle |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2009101163842A CN101503357A (en) | 2009-03-20 | 2009-03-20 | Method for extracting chlorogenic acid in honeysuckle |
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| CN101503357A true CN101503357A (en) | 2009-08-12 |
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| CNA2009101163842A Pending CN101503357A (en) | 2009-03-20 | 2009-03-20 | Method for extracting chlorogenic acid in honeysuckle |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001946A (en) * | 2010-11-11 | 2011-04-06 | 湖南中健欣元生物科技有限公司 | Novel method for simultaneously extracting and separating chlorogenic acid and honeysuckle flower essential oil from honeysuckle flower |
| CN102381974A (en) * | 2011-08-31 | 2012-03-21 | 河南科技大学 | Method for separating and preparing caffeic tannic acid from honeysuckle by utilizing high speed countercurrent chromatography |
| CN102391116A (en) * | 2011-10-05 | 2012-03-28 | 重庆市秀山红星中药材开发有限公司 | Method for extracting chlorogenic acid from honeysuckle flower leaves |
| CN103450019A (en) * | 2013-09-18 | 2013-12-18 | 重庆市中药研究院 | Method for extracting and purifying active components from flower buds and leaves of largeflower-like honeysuckle flower |
| 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 |
| CN104845405A (en) * | 2014-02-17 | 2015-08-19 | 山东禾本堂生物科技有限公司 | Process for extracting honeysuckle dye from honeysuckle |
| CN106362433A (en) * | 2016-08-30 | 2017-02-01 | 江苏康缘药业股份有限公司 | Control method and device of serinus mozambicus mozambicus extract extraction technology |
| CN111450131A (en) * | 2020-05-26 | 2020-07-28 | 四川馥芳集生物科技有限公司 | Method for simultaneously extracting volatile oil and chlorogenic acid from stems and leaves of ligusticum wallichii |
-
2009
- 2009-03-20 CN CNA2009101163842A patent/CN101503357A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102001946A (en) * | 2010-11-11 | 2011-04-06 | 湖南中健欣元生物科技有限公司 | Novel method for simultaneously extracting and separating chlorogenic acid and honeysuckle flower essential oil from honeysuckle flower |
| CN102001946B (en) * | 2010-11-11 | 2014-06-25 | 湖南中健欣元生物科技有限公司 | Novel method for simultaneously extracting and separating chlorogenic acid and honeysuckle flower essential oil from honeysuckle flower |
| CN102381974A (en) * | 2011-08-31 | 2012-03-21 | 河南科技大学 | Method for separating and preparing caffeic tannic acid from honeysuckle by utilizing high speed countercurrent chromatography |
| CN102391116A (en) * | 2011-10-05 | 2012-03-28 | 重庆市秀山红星中药材开发有限公司 | Method for extracting chlorogenic acid from honeysuckle flower leaves |
| CN102391116B (en) * | 2011-10-05 | 2014-03-05 | 重庆市秀山红星中药材开发有限公司 | Method for extracting chlorogenic acid from honeysuckle flower leaves |
| CN103450019A (en) * | 2013-09-18 | 2013-12-18 | 重庆市中药研究院 | Method for extracting and purifying active components from flower buds and leaves of largeflower-like honeysuckle flower |
| CN104845405A (en) * | 2014-02-17 | 2015-08-19 | 山东禾本堂生物科技有限公司 | Process for extracting honeysuckle dye from honeysuckle |
| 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 |
| CN106362433A (en) * | 2016-08-30 | 2017-02-01 | 江苏康缘药业股份有限公司 | Control method and device of serinus mozambicus mozambicus extract extraction technology |
| CN111450131A (en) * | 2020-05-26 | 2020-07-28 | 四川馥芳集生物科技有限公司 | Method for simultaneously extracting volatile oil and chlorogenic acid from stems and leaves of ligusticum wallichii |
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Application publication date: 20090812 |