CN103102270A - Preparation method of chlorogenic acid - Google Patents
Preparation method of chlorogenic acid Download PDFInfo
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- CN103102270A CN103102270A CN2011103618356A CN201110361835A CN103102270A CN 103102270 A CN103102270 A CN 103102270A CN 2011103618356 A CN2011103618356 A CN 2011103618356A CN 201110361835 A CN201110361835 A CN 201110361835A CN 103102270 A CN103102270 A CN 103102270A
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Abstract
The invention relates to a preparation method of chlorogenic acid, belongs to the technical field of medicines, particularly relates to a method for extracting beneficial ingredients from a plant, specifically relates to the preparation method of the chlorogenic acid and provides the preparation method of the chlorogenic acid, which has the advantages of small loss of active ingredients and low cost. The preparation method disclosed by the invention comprises the following steps: crushing honeysuckle flower or caulis lonicerae as raw material, then adding water and stirring to get a water solution; precipitating the water solution with a flocculating agent, and then filtering and colleting supernatant fluid; and separating the supernatant fluid with a membrane, concentrating and drying to get the chlorogenic acid. The process for preparing the chlorogenic acid, disclosed by the invention, adopts a normal-temperature water extraction method, the concentration is performed by a membrane separation system, the loss of the active ingredients is greatly reduced, the content and the yield of a finished product are simultaneously improved, and the consumption and the cost of the raw material are also reduced.
Description
Technical field
The invention belongs to medical technical field, especially a kind of method from the useful composition of plant extract, what be specifically related to is a kind of chlorogenic acid preparation method.
Background content
Chlorogenic acid is coffee and the depside that is generated by coffee and Kui Buddhist nun (QA), a kind of phenylpropanoids that plant materials produces through shikimic acid pathway in the aerobic repiration process, it is the major ingredient of anti-microbial effect in Japanese Honeysuckle and caprifoliaceae plant, its sterling is needle crystal, the hydrophilic solvent such as water-soluble, methyl alcohol, ethanol.Due to the special construction of chlorogenic acid, determined that its utilizable water, ethanol, acetone, methyl alcohol isopolarity solvent extract from plant.After adopting raw material pulverizing mostly, the method for tradition chlorogenic acid extracting uses water extraction, through resin absorption, after ethanol elution, concentrated spray is dry, its shortcoming is in the extraction and concentration process to be to operate at higher temperature, therefore, very large to the destruction of chlorogenic acid, greatly about 30-50%, thereby increased the cost of product.
Summary of the invention
The technical problem to be solved in the present invention is to provide the chlorogenic acid preparation method that a kind of loss of effective components is little, cost is low.
The technical scheme of technical solution problem of the present invention is:
The method of producing chlorogenic acid is take Japanese Honeysuckle or Japanese Honeysuckle Stem as raw material, stirs to get the aqueous solution with adding water after raw material pulverizing; The aqueous solution is collected supernatant liquor with rear filtration of flocculation agent precipitation; With supernatant liquor with membrane sepn after, concentrated, dry chlorogenic acid.
The said raw material pulverizing of method that the present invention produces chlorogenic acid is: raw material powder is broken into 10---40 purpose fine powders.
The present invention produces the said water that adds of the method for chlorogenic acid and stirs and be: add at twice water and stir, amount of water is 10 of raw material weight for the first time---12 times, filter; Amount of water is 6 of raw material weight for the second time---8 times, filter; Merge filtered liquid; Each stirring 2---4 hours.
It is polymerize aluminum chloride with flocculation agent precipitation flocculation agent used that the present invention produces the method for chlorogenic acid said.
The said supernatant liquor membrane sepn of method that the present invention produces chlorogenic acid is: adopting membrane sepn filtrate twice, for ultra-filtration membrane separates, is nanofiltration membrane separation for the first time for the second time.
The method that above-mentioned ultra-filtration membrane separates is: it is 3 that supernatant liquor is transferred pH value---7, be 1KD at molecular weight cut-off---ultrafiltration under the membrane sepn condition of 3KD, pressure-controlling is at 1.5MPa---2.2MPa, temperature is controlled at 20---40 ℃, collect ultrafiltrated.
The method of above-mentioned nanofiltration membrane separation is: it is 3 that ultrafiltrated is transferred pH value---7, being 100D at molecular weight cut-off---under the membrane sepn condition of 300D, nanofiltration is concentrated, pressure-controlling is at 1.5MPa---2.2MPa, and temperature is controlled at 20---40 ℃, collect the nanofiltration concentrated solution.
The present invention produces said concentrated, the drying of the method for chlorogenic acid: it is 1.1 that the nanofiltration concentrated solution is concentrated into proportion---1.2; Drying is spraying drying.
The present invention
The invention has the beneficial effects as follows:
1, the present invention produces the method for chlorogenic acid, and after adopting normal-temperature water to stir extraction, through flocculation agent precipitation, overanxious, with membrane sepn, concentrate drying, because technological process is produced under the lower condition of temperature all the time, so the loss of the effective ingredient chlorogenic acid in raw material is few.
2, the present invention produce in the procedure of chlorogenic acid with after a raw material of pulverizing added water stirring with the flocculation agent precipitation, filter, can remove and stir the impurity that suspends in liquid, also reduced the loss of active ingredient chlorogenic acid.
3, the present invention produces the method employing membrane sepn of chlorogenic acid, the effect of twice separation is, passing through 1KD---the supermembrane of 3KD is removed the content of the macromole impurity raising solution Content of Chlorogenic Acid in extracting solution, passing through 100D---the film of receiving of 300D is further removed the small molecular weight impurities such as inorganic salt in solution, heavy metal, so the content of chlorogenic acid in solution has also and gets a greater increase.
4, the present invention produces the method for chlorogenic acid, under normal temperature, concentrated solution is 1.1 to proportion---1.2, to reduce the loss of chlorogenic acid under the concentrated condition of heat, concentrated solution can get content by spraying drying and be not less than 40% chlorogenic acid dry powder, and extraction yield is higher than 90%.
Compared with prior art, the technique that the present invention produces chlorogenic acid is to adopt the normal-temperature water formulation, and is concentrated through film separating system, greatly reduced loss of effective components, improves simultaneously finished product content and yield, reduced raw material consumption and cost.
Embodiment
Below in conjunction with embodiment, the present invention is described in further details.
Embodiment 1:
1, extracting honeysuckle 100kg, be ground into 10---40 purpose fine powders, add water and stir extraction twice, add for the first time 10 times of amounts of water, stir after 2 hours and filter, add for the second time 6 times of amounts of water, stirred 3 hours, and filtered, pH value transfers to 7, merge extracted twice liquid polyaddition aluminum chloride flocculant precipitation, cross the leaching supernatant liquor;
2, supernatant liquor being transferred pH value is 7, is 1KD at molecular weight cut-off---ultrafiltration under the ultra-filtration membrane separation condition of 3KD, and pressure-controlling is at 1.5MPa---2.2MPa, temperature is controlled at 20---40 ℃, collect ultrafiltrated;
3, ultrafiltrated being transferred pH value is 6, it is nanofiltration under the membrane sepn condition of 100D at molecular weight cut-off, pressure-controlling is at 1.5MPa---2.2MPa, temperature is controlled at 20---and 40 ℃, concentrated nanofiltration liquid to proportion is 1.1---1.2, spraying drying gets dry powder 13.22kg, and chlorogenic acid content is 40.9%, is 91.7% by medicinal material content meter yield.
Embodiment 2:
1, get Japanese Honeysuckle Stem 100kg, be ground into 10---40 purpose fine powders, add water and stir extraction twice, add for the first time 12 times of amounts of water, stir after 3 hours and filter, add for the second time 8 times of amounts of water, stirred 4 hours, pH value transfers to 3, merges extracted twice liquid polyaddition aluminum chloride flocculant precipitation, crosses the leaching supernatant liquor;
2, supernatant liquor being transferred pH value is 5, is ultrafiltration under the membrane sepn condition of 3KD at molecular weight cut-off, and pressure-controlling is at 1.0MPa---2.2MPa, and temperature is controlled at 20---40 ℃, collect ultrafiltrated;
3, ultrafiltrated being transferred pH value is 6, it is nanofiltration under the membrane sepn condition of receiving of 300D at molecular weight cut-off, pressure-controlling is at 1.5MPa---2.2MPa, temperature is controlled at 20---and 40 ℃, concentrated nanofiltration liquid to proportion is 1.1---1.2, spraying drying gets dry powder 5.81kg, and chlorogenic acid content is 41.2%, is 90.3% by medicinal material content meter yield.
KD in preparation method of the present invention is kilodalton unit.
Claims (8)
1. chlorogenic acid preparation method is characterized in that: take Japanese Honeysuckle or Japanese Honeysuckle Stem as raw material, stir to get the aqueous solution with adding water after raw material pulverizing; The aqueous solution is collected supernatant liquor with rear filtration of flocculation agent precipitation; With supernatant liquor with membrane sepn after, concentrated, dry chlorogenic acid.
2. said preparation method according to claim 1, it is characterized in that: said raw material pulverizing is that raw material powder is broken into 10---40 purpose fine powders.
3. said preparation method according to claim 1 is characterized in that: the said water that adds stirs and is: add at twice water and stir, amount of water is 10 of raw material weight for the first time---12 times, filter; Amount of water is 6 of raw material weight for the second time---8 times, filter; Merge filtered liquid; Each stirring 2---4 hours.
4. said preparation method according to claim 1, it is characterized in that: said is polymerize aluminum chloride with flocculation agent precipitation flocculation agent used.
5. said preparation method according to claim 1, it is characterized in that: said supernatant liquor membrane sepn is: adopting membrane sepn filtrate twice, for ultra-filtration membrane separates, is nanofiltration membrane separation for the first time for the second time.
6. said preparation method according to claim 5, it is characterized in that: the method that described ultra-filtration membrane separates is: it is 3 that supernatant liquor is transferred pH value---7, be 1KD at molecular weight cut-off---ultrafiltration under the membrane sepn condition of 3KD, pressure-controlling is at 1.5MPa---2.2MPa, temperature is controlled at 20---40 ℃, collect ultrafiltrated.
7. said preparation method according to claim 5, it is characterized in that: the method for described nanofiltration membrane separation is: it is 3 that ultrafiltrated is transferred pH value---7, be 100D at molecular weight cut-off---ultrafiltration under the membrane sepn condition of 300D, pressure-controlling is at 1.5MPa---2.2MPa, temperature is controlled at 20---40 ℃, collect the nanofiltration concentrated solution.
8. said preparation method according to claim 1 is characterized in that: said concentrated, drying is that the nanofiltration concentrated solution is concentrated into proportion is 1.1---1.2; Drying is spraying drying.
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| CN2011103618356A CN103102270A (en) | 2011-11-09 | 2011-11-09 | Preparation method of chlorogenic acid |
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| CN2011103618356A CN103102270A (en) | 2011-11-09 | 2011-11-09 | Preparation method of chlorogenic acid |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103494738A (en) * | 2013-09-29 | 2014-01-08 | 上海莱博生物科技有限公司 | Method for preparing natural antiseptic traditional Chinese medicine compound extract |
| CN104542587A (en) * | 2014-12-18 | 2015-04-29 | 昆明理工大学 | Application of chlorogenic acid in relieving of aluminum toxicity in soybean seedlings |
| CN105497101A (en) * | 2015-12-16 | 2016-04-20 | 张家界立功旅游农业发展有限公司 | Method for extracting kinds of combined extract from blueberry stems and leaves |
| CN109970564A (en) * | 2019-04-26 | 2019-07-05 | 安徽科博瑞环境科技有限公司 | The extracting method of Chlorogenic Acid of Flos Lonicerae |
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| JPS60243016A (en) * | 1984-05-17 | 1985-12-03 | Tsumura Juntendo Inc | Anti-influenza virus agent |
| CN1247836A (en) * | 1998-09-15 | 2000-03-22 | 滕赪伟 | Preparation of clear water containing honeysuckle flower component |
| US6083921A (en) * | 1998-01-12 | 2000-07-04 | Xu; Kai Jian | Pharmaceutical compositions and method of using same |
| CN1810763A (en) * | 2005-01-28 | 2006-08-02 | 李全才 | Honeysuckle chlorogenic acid extracting technology |
| KR20090089660A (en) * | 2008-02-19 | 2009-08-24 | 환인제약 주식회사 | Composition comprising the extract of lonicera japonica thunb. preventing and treating arthritis |
| CN101530449A (en) * | 2008-01-22 | 2009-09-16 | 上海中药制药技术有限公司 | Method of preparing honeysuckle extract by applying membrane filtration technology |
| 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 |
-
2011
- 2011-11-09 CN CN2011103618356A patent/CN103102270A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS60243016A (en) * | 1984-05-17 | 1985-12-03 | Tsumura Juntendo Inc | Anti-influenza virus agent |
| US6083921A (en) * | 1998-01-12 | 2000-07-04 | Xu; Kai Jian | Pharmaceutical compositions and method of using same |
| CN1247836A (en) * | 1998-09-15 | 2000-03-22 | 滕赪伟 | Preparation of clear water containing honeysuckle flower component |
| CN1810763A (en) * | 2005-01-28 | 2006-08-02 | 李全才 | Honeysuckle chlorogenic acid extracting technology |
| CN101530449A (en) * | 2008-01-22 | 2009-09-16 | 上海中药制药技术有限公司 | Method of preparing honeysuckle extract by applying membrane filtration technology |
| KR20090089660A (en) * | 2008-02-19 | 2009-08-24 | 환인제약 주식회사 | Composition comprising the extract of lonicera japonica thunb. preventing and treating arthritis |
| 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 |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103494738A (en) * | 2013-09-29 | 2014-01-08 | 上海莱博生物科技有限公司 | Method for preparing natural antiseptic traditional Chinese medicine compound extract |
| CN104542587A (en) * | 2014-12-18 | 2015-04-29 | 昆明理工大学 | Application of chlorogenic acid in relieving of aluminum toxicity in soybean seedlings |
| CN104542587B (en) * | 2014-12-18 | 2016-06-08 | 昆明理工大学 | Chlorogenic acid application in alleviating soybean seedling aluminium toxicity |
| CN105497101A (en) * | 2015-12-16 | 2016-04-20 | 张家界立功旅游农业发展有限公司 | Method for extracting kinds of combined extract from blueberry stems and leaves |
| CN109970564A (en) * | 2019-04-26 | 2019-07-05 | 安徽科博瑞环境科技有限公司 | The extracting method of Chlorogenic Acid of Flos Lonicerae |
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Application publication date: 20130515 |