CN102391116A - Method for extracting chlorogenic acid from honeysuckle flower leaves - Google Patents
Method for extracting chlorogenic acid from honeysuckle flower leaves Download PDFInfo
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- CN102391116A CN102391116A CN2011102926985A CN201110292698A CN102391116A CN 102391116 A CN102391116 A CN 102391116A CN 2011102926985 A CN2011102926985 A CN 2011102926985A CN 201110292698 A CN201110292698 A CN 201110292698A CN 102391116 A CN102391116 A CN 102391116A
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Abstract
The invention relates to a method for extracting chlorogenic acid from honeysuckle flower leaves. The method comprises the following steps of: crushing, soaking, filtering, eluting, concentrating, drying, packaging in separate bags and the like. By the method, effective resources are utilized to a maximum limit, economic benefit is increased, food grade ethanol is used as an extractant and a purifying agent in the production process, and the chlorogenic acid is extracted at normal temperature, so the production cost is reduced, and the chlorogenic acid is prevented from being decomposed; the honeysuckle flower leaves are soaked for multiple times in the soaking process, and extraction solution is obtained, so the purity is improved effectively; and purification and elution are performed by using macroporous resin, so that the purity of the chlorogenic acid is improved greatly to 35 to 95 percent according to requirements.
Description
Technical field
The present invention relates to a kind of method of chlorogenic acid extracting, particularly a kind of from leaf of Flos Lonicerae the method for chlorogenic acid extracting.
Background technology
Japanese Honeysuckle belongs to caprifoliaceae plant, and herb all can be used as medicine, and bud contains volatile aromatic oil, inositol, saponin(e, chlorogenicacid, flavonoid compound, styracin, vernol, Mo Liquan etc., contains vegeto-alkali in the stem; Containing lonicerin and sweet-scented osmanthus element etc. in the leaf, is one of traditional Chinese medicine material, also is the raw material of medicine-food two-purpose, has clearing heat and detoxicating; Wind-heat dissipating, the effect of hepatic cholagogic is used for the swollen furunculosis of carbuncle, larynx numbness always in traditional Chinese medical science field; Erysipelas, toxic-heat and blood stasis, common cold due to wind-heat, the treatment of warm morbidity; Particularly all contain chlorogenicacid in gold and silver bud, stem, the leaf, chlorogenicacid has good effect to preventing and treating upper respiratory tract infection, common cold due to wind-heat and gastroenteropathy, to removing human free radical, delaying senility, improve human immunologic function etc. and have good effect; Thereby chlorogenic acid extracting is the important topic of pharmacy field, and traditional chlorogenicacid extraction process is chlorogenic acid extracting from Japanese Honeysuckle only mostly, has ignored the extraction of chlorogenicacid in the cauline leaf, serious waste efficient resource.
Summary of the invention
Technical problem to be solved by this invention provides a kind of method of utilizing the leaf of Flos Lonicerae chlorogenic acid extracting, to obtain efficient resource to greatest extent, cuts the waste.
For solving the problems of the technologies described above, the technical scheme that the present invention adopted by pulverizing, immersion, filtration, wash-out, concentrate, dry, packing forms, and is specific as follows.
⑴ pulverize: leaf of Flos Lonicerae is clean, dry, pulverizing, the powder size is 20～40 orders.
⑵ soak: divides and soak and extract and filtrate for three times, and merging filtrate then, operation steps is following:
For the first time: powder is immersed in the ethanolic soln, and alcohol concn is 65～75%, and solid-to-liquid ratio is 1kg:8～10L, and soak time 45～55min filters and obtains extracting solution, stays filter residue;
For the second time: again filter residue being added concentration is 65～75% ethanol, 10～12L, soaks 35～45min, filters and obtains extracting solution, stays filter residue;
For the third time: the concentration of filter residue adding for the second time is 65～75% ethanol, 8～10L, soaks 30-40min, filters and obtains extracting solution; The extracting solution that merges three times then is for use.
⑶ filter: in extracting solution, add finings, left standstill 10～14 hours after fully stirring, and the albumen in the precipitation solution, tannin, natural gum and impurity, separation of supernatant and throw out filter then and obtain supernatant filtrating.
⑷ wash-out: with macroporous resin adsorption supernatant filtrating, flow rate control is at 400～600L/hr; Use the purified water wash-out then, flow rate control is 300～500L/hr, and the overall control of purified water elutriant is about 0.5～1 times of resin volume, discards elutriant; Use again that pH value is 2～3, concentration is 45～65% ethanolic soln wash-out, flow rate control is at 400～600L/hr, elutriant (50% ethanol) overall control is about 3 times of resin volumes, reclaims the elutriant that contains chlorogenicacid at last.
⑸ concentrate: the elutriant that will contain chlorogenicacid is concentrated into the liquid concentrator that specific density is 1.15～1.20 (50 ℃ of surveys) through nanofiltration.
⑹ dry: suck through the spissated liquid concentrator of nanofiltration thickening equipment through vacuum; Vacuum tightness is that 0.01～0.08Mpa, drying temperature are controlled at (keep water tank temperature at 85～95 ℃, the charging stock tank temperature is controlled at 45～65 ℃), input speed 180～200mm/min below 60 ℃; And receive the powder middle turning barrel of packing into, weighing is sticked bucket and is signed, place material temporary between, the censorship intermediates.
⑺ packing: after treating these article check qualified (moisture≤8.0%, bacterium must not be more than 800/g, containing mould must not be more than 80/g, escherichia coli must not detect), clean rank be between 100,000 grades clean packaging in packing; Changing shady and cool storehouse (18～26 ℃ of temperature, relative humidity 45～75%) over to preserves.
The present invention has utilized efficient resource to greatest extent, has increased economic benefit, uses food grade ethanol as extraction agent and purifying agent in process of production; And extract at normal temperatures, can reduce production costs, avoid chlorogenicacid to decompose; In immersion process, repeatedly soak and get liquid, improved purity effectively, purify and wash-out with macroporous resin then; Improved the purity of chlorogenicacid greatly, as required, can make the 35-95% that reaches of chlorogenicacid purity.
Description of drawings
Accompanying drawing is the process flow sheet of the present invention's method of chlorogenic acid extracting from leaf of Flos Lonicerae.
Embodiment
Below in conjunction with embodiment the present invention is described further.
The dry leaf of Flos Lonicerae 10kg that will pass through after the roughing pulverizes, and crosses sieve No. four; Then powder is immersed in the 100L ethanolic soln, alcohol concn is 70%, and soak time 50min filters and obtains extracting solution, stays filter residue; Then filter residue being added concentration is 70% ethanol 110L, soaks 40min, filters and obtains extracting solution, stays filter residue; Then the concentration of filter residue adding for the second time is 70% ethanol 90L, soaks 35min, filters and obtains extracting solution; The extracting solution that merges three times then is for use.
In extracting solution, add finings, left standstill 12 hours after fully stirring, separation of supernatant and throw out filter then and obtain supernatant filtrating; Use particle diameter as the macroporous resin of 0.8mm supernatant to be adsorbed supernatant filtrating again, flow velocity is 500L/hr; Use the purified water wash-out then, flow velocity is 400L/hr, and purified water elutriant total amount is 1 times of resin volume, discards elutriant; Use again that pH value is 2.5, concentration is 55% ethanolic soln wash-out, flow velocity is 500L/hr, elutriant (50% ethanol) is 3 times of resin volumes, reclaims the elutriant that contains chlorogenicacid at last.
The elutriant that will contain chlorogenicacid is concentrated into the liquid concentrator that specific density is 1.15 (50 ℃ of surveys) through nanofiltration; Suck through the spissated liquid concentrator of nanofiltration thickening equipment through vacuum then; Vacuum tightness is that 0.05Mpa, drying temperature are controlled to be 55 ℃ (keeping water tank temperature is 90 ℃, and the charging stock tank temperature is controlled to be 60 ℃), input speed 190mm/min; And receive the powder middle turning barrel of packing into, weighing is sticked bucket and is signed, place material temporary between, inspect intermediates again by ready samples.
(moisture≤8.0% will be up to the standards; Bacterium must not be more than 800/g; Containing mould must not be more than 80/g; Escherichia coli must not detect) product be placed on clean rank be between 100,000 grades clean packaging in packing, change shady and cool storehouse (18～26 ℃ of temperature, relative humidity 45～75%) then over to and preserve.
Claims (3)
1. the method for chlorogenic acid extracting from leaf of Flos Lonicerae, by pulverizing, immersion, filtration, wash-out, concentrate, drying and packing step form, and it is characterized in that concrete steps are following:
⑴ pulverize: leaf of Flos Lonicerae is clean, dry, pulverizing, cross sieve No. four;
⑵ soak: divide and soak and extract filtrating, merging filtrate then three times;
⑶ filter: in extracting solution, add finings, left standstill 10～14 hours after fully stirring, and the albumen in the precipitation solution, tannin, natural gum and impurity, separation of supernatant and throw out filter then and obtain supernatant filtrating;
⑷ wash-out: with macroporous resin adsorption supernatant filtrating, flow rate control is at 400～600L/hr; Use the purified water wash-out then, flow rate control is 300～500L/hr, and the overall control of purified water elutriant is about 0.5～1 times of resin volume, discards elutriant; Use again that pH value is 2～3, concentration is 45～65% ethanolic soln wash-out, flow rate control is at 400～600L/hr, elutriant (50% ethanol) overall control is about 3 times of resin volumes, reclaims the elutriant that contains chlorogenicacid at last;
⑸ concentrate: the elutriant that will contain chlorogenicacid is concentrated into the liquid concentrator that specific density is 1.15～1.20 (50 ℃ of surveys) through nanofiltration;
⑹ dry: suck liquid concentrator through vacuum and carry out drying, obtain the chlorogenicacid powder, collect the chlorogenicacid powder and the middle turning barrel of packing into, weighing is sticked bucket and is signed, place material temporary between, the censorship intermediates;
⑺ packing: treat that the chlorogenicacid powder is up to the standards after (moisture≤8.0%, bacterium must not be more than 800/g, containing mould must not be more than 80/g, escherichia coli must not detect), clean rank be between 100,000 grades clean packaging in packing; Changing shady and cool storehouse (18～26 ℃ of temperature, relative humidity 45～75%) at last over to preserves.
2. according to claim 1 from leaf of Flos Lonicerae the method for chlorogenic acid extracting, it is characterized in that the described immersion of step ⑵ is meant that branch soaks for three times and extracts filtrating, merging filtrate then, the concrete operations step is following:
⑴ for the first time: powder is immersed in the ethanolic soln, and alcohol concn is 65～75%, and solid-to-liquid ratio is 1kg:8～10L, and soak time 45～55min filters and obtains extracting solution, stays filter residue;
⑵ for the second time: again filter residue being added concentration is 65～75% ethanol, 10～12L, soaks 35～45min, filters and obtains extracting solution, stays filter residue;
⑶ for the third time: to add concentration is 65～75% ethanol, 8～10L to filter residue for the second time, soaks 30-40min, filters and obtains extracting solution;
⑷ the extracting solution that merging is three times is for use.
3. according to claim 1 from leaf of Flos Lonicerae the method for chlorogenic acid extracting; It is characterized in that the described drying of step ⑹ is meant that sucking liquid concentrator through vacuum carries out drying; Vacuum tightness is that 0.01～0.08Mpa, drying temperature are controlled at below 60 ℃ (keep water tank temperature at 85～95 ℃, the charging stock tank temperature is controlled at 45～65 ℃), input speed is 180～200mm/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104844458A (en) * | 2014-02-17 | 2015-08-19 | 山东禾本堂生物科技有限公司 | Process for extracting chlorogenic acid and dye from honeysuckle leaf |
| CN104905099A (en) * | 2015-05-20 | 2015-09-16 | 江西思科食品有限公司 | Blueberry jam and preparation method thereof |
| CN106431929A (en) * | 2016-08-31 | 2017-02-22 | 湖北山鼎环境科技股份有限公司 | Method for extracting chlorogenic acid from honeysuckle and intelligent control system |
| WO2024031997A1 (en) * | 2022-08-11 | 2024-02-15 | 山东省分析测试中心 | N-n-bis-oxazolidinone alkaloid compounds, preparation method, and use in medical field |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250106A (en) * | 2008-03-27 | 2008-08-27 | 北京市农林科学院 | Method for extracting chlorogenic acid |
| CN101503357A (en) * | 2009-03-20 | 2009-08-12 | 安徽省祁门“黄山药谷”生物科技有限公司 | Method for extracting chlorogenic acid in honeysuckle |
| CN101838200A (en) * | 2009-03-20 | 2010-09-22 | 上海中医药大学 | Method for extracting and separating chlorogenic acid from honeysuckle |
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2011
- 2011-10-05 CN CN201110292698.5A patent/CN102391116B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101250106A (en) * | 2008-03-27 | 2008-08-27 | 北京市农林科学院 | Method for extracting chlorogenic acid |
| CN101503357A (en) * | 2009-03-20 | 2009-08-12 | 安徽省祁门“黄山药谷”生物科技有限公司 | Method for extracting chlorogenic acid in honeysuckle |
| CN101838200A (en) * | 2009-03-20 | 2010-09-22 | 上海中医药大学 | Method for extracting and separating chlorogenic acid from honeysuckle |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN104844458A (en) * | 2014-02-17 | 2015-08-19 | 山东禾本堂生物科技有限公司 | Process for extracting chlorogenic acid and dye from honeysuckle leaf |
| CN104905099A (en) * | 2015-05-20 | 2015-09-16 | 江西思科食品有限公司 | Blueberry jam and preparation method thereof |
| CN106431929A (en) * | 2016-08-31 | 2017-02-22 | 湖北山鼎环境科技股份有限公司 | Method for extracting chlorogenic acid from honeysuckle and intelligent control system |
| CN106431929B (en) * | 2016-08-31 | 2019-08-16 | 湖北工业职业技术学院 | The method and intelligence control system of extracting chlorogenci acid from honeysuckle |
| WO2024031997A1 (en) * | 2022-08-11 | 2024-02-15 | 山东省分析测试中心 | N-n-bis-oxazolidinone alkaloid compounds, preparation method, and use in medical field |
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| CN102391116B (en) | 2014-03-05 |
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