CN1435406A - Process for preparing chlorogenic acid - Google Patents
Process for preparing chlorogenic acid Download PDFInfo
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- CN1435406A CN1435406A CN 03111946 CN03111946A CN1435406A CN 1435406 A CN1435406 A CN 1435406A CN 03111946 CN03111946 CN 03111946 CN 03111946 A CN03111946 A CN 03111946A CN 1435406 A CN1435406 A CN 1435406A
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- chlorogenic acid
- organic solvent
- arctii leaf
- herba arctii
- crude extract
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Abstract
A process for preparing the chlorogenic acid used as medicinal component includes reflux extraction of dried arctium leaves in organic solvent at pH=2-3 several times for 3 hr, filtering per time, collecting filtrate, vacuum concentrating, recovering alcohol to obtain raw extract, chromatography by polyamide column, eluting with water and methanol, concentrating and refining. Its advantage is low cost.
Description
(1) technical field
The present invention relates to a kind of extracting method of plants ' medicinal component, specifically, be a kind of be the method for feedstock production chlorogenic acid with Herba Arctii leaf cheaply.
(2) background technology
Chlorogenic acid (chlorogenic acid) belongs to the caffeoyl guinic acid class, resistance of oxidation is strong, the functions such as activity that also have AIDS resisting poison, tumor cell line cytotoxic activity, teratogenesis, antianaphylaxis and regulate the enzyme of Cytochrome P450 connection, chlorogenic acid all is a kind of important component in medicines such as numerous anti-common cold poison, uses very extensive.Chlorogenic acid is described as " plant gold ", is the object that production is chased by numerous producers.The domestic production chlorogenic acid is a raw material with Japanese Honeysuckle, the bark of eucommia etc. mainly, is raw material with coffee berry etc. mainly abroad, and starting material are restricted unavoidably, and cost is higher.
Feverfew burdock (Arctium lappa L.) has been realized large-area artificial culture in China, mainly utilizes its root, goes out of use substantially but annual a large amount of Herba Arctii leaf is taken as refuse, and causes certain environmental pollution.By conservative estimation Shandong, the 200000 mu of burdock planting sites in two places, Jiangsu, every per mu yield 200Kg Herba Arctii leaf calculates, and can produce 40000 tons of Herba Arctii leaf per year.Experiment shows the chlorogenic acid that contains high level in the Herba Arctii leaf, if can make full use of these Herba Arctii leaf refuses, will reduce the production cost of chlorogenic acid greatly, but not see the open report of this respect up to now.
(3) summary of the invention
At the deficiencies in the prior art, the invention provides a kind of is the method for feedstock production chlorogenic acid with Herba Arctii leaf.
Technical scheme of the present invention is as follows:
A kind of method for preparing chlorogenic acid comprises with organic solvent the raw material refluxing extraction, suction filtration, and merging filtrate, filtrate decompression concentrates and the separation and purification of crude extract, and raw materials used is dried Herba Arctii leaf.
Above-mentioned organic solvent is the acid solution of low-carbon (LC) straight or branched alcohol of pH2～3, carbon number 1～5, and as ethanol, propyl alcohol, methyl alcohol, butanols, the mixing of one of them or they such as ethylene glycol.
It is 2～4 times that dried Herba Arctii leaf is extracted in above-mentioned organic solvent gradation.
The above-mentioned dried Herba Arctii leaf and the consumption of organic solvent are: dried Herba Arctii leaf 100～150g, organic solvent 2000～3000ml.
The aforesaid method concrete operations are as follows:
With the dried Herba Arctii leaf 3h of organic solvent solution gradation refluxing extraction of pH2～3, reflux temperature is with reference to the boiling point of organic solvent, as being 76～80 ℃ with the alcohol reflux temperature, each back suction filtration that extracts, merging filtrate, filtrate decompression concentrates, reclaim organic solvent, get the Herba Arctii leaf crude extract.
Dried Herba Arctii leaf is extracted in above-mentioned organic solvent gradation, the 1st 1～2h, the 2nd 1～1.5h, the 3rd 0.5～1h, the 4th 0.5h.
At last, above-mentioned Herba Arctii leaf crude extract is crossed polyamide column, water and methanol-eluted fractions, elutriant gets the pure product of chlorogenic acid through concentrating, making with extra care.
Analyze and standard control through RP-HPLC, UV, LC-ESI-MS, show in the above-mentioned Herba Arctii leaf crude extract to contain chlorogenic acid, and chlorogenic acid a kind of main component in the Herba Arctii leaf crude extract for this reason.Further separation and purification can get the pure product of chlorogenic acid.
The present invention is a kind of Herba Arctii leaf source new drugs for chlorogenic acid production has searched out.Well imagine that it is very cheap that Herba Arctii leaf is made material cost, will reduce the total cost of production of chlorogenic acid greatly, and working method is simple.
(4) embodiment
Embodiment 1:
The indoor natural airing of fresh Herba Arctii leaf divides 2 inferior to 78 ℃ of dried Herba Arctii leaf of refluxing extraction 100g with 2000ml ethanol (pH2), the 1st 2h, and the 2nd 1h extracts the back suction filtration at every turn, merging filtrate, filtrate decompression concentrates, and reclaims ethanol, gets the Herba Arctii leaf crude extract.Through analysis and standard controls such as RP-HPLC, UV, LC-ESI-MS, show to contain chlorogenic acid in this Herba Arctii leaf crude extract, and chlorogenic acid a kind of main component in the Herba Arctii leaf crude extract for this reason.
Embodiment 2:
Dried Herba Arctii leaf divides 3 inferior to 77 ℃ of dried Herba Arctii leaf of refluxing extraction 150g with 3000ml ethanol (pH3), the 1st 1h, the 2nd 1h, the 3rd 1h.Extract the back suction filtration at every turn, merging filtrate, filtrate decompression concentrates, and reclaims ethanol, gets the Herba Arctii leaf crude extract.Through analysis and standard controls such as RP-HPLC, UV, LC-ESI-MS, show to contain chlorogenic acid in this Herba Arctii leaf crude extract, and chlorogenic acid a kind of main component in the Herba Arctii leaf crude extract for this reason.The Herba Arctii leaf crude extract is crossed polyamide column, water and methanol-eluted fractions, elutriant gets the pure product of chlorogenic acid through concentrating, making with extra care.
Embodiment 3:
Dried Herba Arctii leaf divides 4 inferior to 79 ℃ of dried Herba Arctii leaf of refluxing extraction 150g with 2500ml ethanol (pH2.5), the 1st 1h, the 2nd 1h, the 3rd 0.5h, the 4th 0.5h.Extract the back suction filtration at every turn, merging filtrate, filtrate decompression concentrates, and reclaims ethanol, gets the Herba Arctii leaf crude extract.Through analysis and standard controls such as RP-HPLC, UV, LC-ESI-MS, show to contain chlorogenic acid in this Herba Arctii leaf crude extract, and chlorogenic acid a kind of main component in the Herba Arctii leaf crude extract for this reason.The Herba Arctii leaf crude extract is crossed polyamide column, water and methanol-eluted fractions, elutriant gets the pure product of chlorogenic acid through concentrating, making with extra care.
Embodiment 4:
As described in embodiment 1, different is that organic solvent is methyl alcohol and 1: 1 the mixed solution of ethanol of pH2.5.
Embodiment 5:
As described in embodiment 1, different is that organic solvent is the ethylene glycol of pH3.
Embodiment 6:
As described in embodiment 2, different is that organic solvent is the butanols of pH2.
Embodiment 7:
As described in embodiment 2, different is that organic solvent is ethanol and 2: 1 the mixed solution of propyl alcohol of pH2.5.
Embodiment 8:
As described in embodiment 3, different is that organic solvent is the propyl alcohol of pH2.
Claims (6)
1. method for preparing chlorogenic acid comprises with organic solvent the raw material refluxing extraction, suction filtration, and merging filtrate, filtrate decompression concentrates and the crude extract separation and purification, it is characterized in that the raw materials used dried Herba Arctii leaf that is.
2. the method for preparing chlorogenic acid as claimed in claim 1 is characterized in that, above-mentioned organic solvent is the acid solution of low-carbon (LC) straight or branched alcohol of pH2～3, and carbon number 1～5 comprises the mixing of ethanol, propyl alcohol, methyl alcohol, butanols, ethylene glycol one of them or they.
3. the method for preparing chlorogenic acid as claimed in claim 1 is characterized in that, the above-mentioned dried Herba Arctii leaf and the consumption of organic solvent are: dried Herba Arctii leaf 100～150g, organic solvent 2000～3000ml.
4. as claim 1 or the 2 or 3 described methods that prepare chlorogenic acid, it is characterized in that the dried Herba Arctii leaf of described organic solvent extraction is 2～4 times.
5. the method for preparing chlorogenic acid as claimed in claim 1 or 2 is characterized in that, dried Herba Arctii leaf is extracted in described organic solvent gradation, the 1st 1～2hr, the 2nd 1～1.5hr, the 3rd 0.5～1hr; The 4th 0.5hr.
6. the method for preparing chlorogenic acid as claimed in claim 1 is characterized in that concrete operations are as follows:
With the dried Herba Arctii leaf 3h of organic solvent solution gradation refluxing extraction of pH2～3, extract the back suction filtration at every turn, merging filtrate, filtrate decompression concentrates, and reclaims organic solvent, gets the Herba Arctii leaf crude extract;
At last, the Herba Arctii leaf crude extract is crossed polyamide column, water and methanol-eluted fractions, elutriant gets the pure product of chlorogenic acid through concentrating, making with extra care.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03111946 CN1435406A (en) | 2003-03-06 | 2003-03-06 | Process for preparing chlorogenic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 03111946 CN1435406A (en) | 2003-03-06 | 2003-03-06 | Process for preparing chlorogenic acid |
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| CN1435406A true CN1435406A (en) | 2003-08-13 |
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| CN 03111946 Pending CN1435406A (en) | 2003-03-06 | 2003-03-06 | Process for preparing chlorogenic acid |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326827C (en) * | 2005-01-13 | 2007-07-18 | 付信君 | Production technology of extracting chlorogenic acid from burdock leaf |
| 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 |
| CN112391397A (en) * | 2020-11-25 | 2021-02-23 | 云南中烟工业有限责任公司 | Tobacco flavone monooxygenase gene NtCYP75B2 and application thereof |
-
2003
- 2003-03-06 CN CN 03111946 patent/CN1435406A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1326827C (en) * | 2005-01-13 | 2007-07-18 | 付信君 | Production technology of extracting chlorogenic acid from burdock leaf |
| 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 |
| CN112391397A (en) * | 2020-11-25 | 2021-02-23 | 云南中烟工业有限责任公司 | Tobacco flavone monooxygenase gene NtCYP75B2 and application thereof |
| CN112391397B (en) * | 2020-11-25 | 2023-01-31 | 云南中烟工业有限责任公司 | Tobacco flavone monooxygenase gene NtCYP75B2 and application thereof |
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