CN102911055B - Method for extracting chlorogenic acid - Google Patents
Method for extracting chlorogenic acid Download PDFInfo
- Publication number
- CN102911055B CN102911055B CN201210453316.7A CN201210453316A CN102911055B CN 102911055 B CN102911055 B CN 102911055B CN 201210453316 A CN201210453316 A CN 201210453316A CN 102911055 B CN102911055 B CN 102911055B
- Authority
- CN
- China
- Prior art keywords
- chlorogenic acid
- column
- ethanol
- supernatant liquor
- extraction
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for extracting a chlorogenic acid. The method includes the following steps of smashing honeysuckle, soaking smashed honeysuckle by ethanol or water, then performing wall-breaking extraction through ultrasound, microwave or enzyme, performing ethanol extraction to obtain a coarse extract, then concentrating the obtained coarse extract to obtain an extractum, adding water to dissolve the extractum to obtain supernatant, then adding the supernatant in a resin adsorbing column, washing by water, washing the column by a 10% to 50% (v/v) ethanol solution, collecting an eluant, enabling the eluant to pass through an activated charcoal column, and collecting a liquid to obtain the chlorogenic acid. The method for extracting the chlorogenic acid has the advantages that the preparation process is simple, the cost is low, the extraction efficiency of the chlorogenic acid is high, the content of the chlorogenic acid in prepared product is high, and the industrialized production is facilitated.
Description
Technical field
The present invention relates to a kind of technique, particularly the method for chlorogenic acid extracting.
Background technology
Japanese Honeysuckle belongs to caprifoliaceae plant, has clearing heat and detoxicating effect, be China conventional be also one of historical longer Chinese medicine.Be used for clinically treating diseases caused by dampness heating, the various diseases such as common cold due to wind-heat.Chlorogenic acid is one of effective constituent in Japanese Honeysuckle, there is multiple pharmacologically active as removed free radical, antisepsis and anti-inflammation, antiviral etc., therefore chlorogenic acid is more and more subject to medicine scholars' attention, and modern science has been deep into multiple fields such as food, health care, medicine and daily-use chemical industry to the research of chlorogenic acid pharmacologically active.
Itself has unstable chlorogenic acid, when extraction, will avoid high temperature, long-time heating and strong illumination.From Japanese Honeysuckle, the traditional method of chlorogenic acid extracting has decocting cooking method, water extraction and alcohol precipitation method, rare alcohol reflux method, supercritical CO
2extraction process, percolation etc.Supercritical CO
2extraction process solvent is easy to get, and productive rate is high, but cost is also high, also there is no at present large-scale application in suitability for industrialized production.Percolation extraction efficiency is higher, but consuming time longer, and economic benefit is not high.The method of tradition separation and purification chlorogenic acid mainly contains extraction process, alkaline precipitation, Thin-layer chromatography, macroreticular resin absorbing method etc., alkaline precipitation easily makes chlorogenic acid hydrolysis, extraction rule needs a large amount of organic solvents, and Thin-layer chromatography and macroreticular resin absorbing method cost are higher, are unfavorable for suitability for industrialized production.
Summary of the invention
One of object of the present invention is to provide the method for chlorogenic acid extracting, and technique is simple, and cost is low, and extraction efficiency is high, and the chlorogenic acid purity making is high, is convenient to suitability for industrialized production.
For achieving the above object, technical scheme is:
The method of chlorogenic acid extracting, comprises the steps:
A. after Japanese Honeysuckle being pulverized, by alcohol immersion, then broken wall lixiviate, makes crude extract;
B. step a gained crude extract is concentrated into medicinal extract, after being dissolved in water, gets supernatant liquor;
C. step b gained supernatant liquor is added in resin absorbing column, after water rinses, then wash post with the ethanolic soln that volume fraction is 10% ~ 50%, collect elutriant, elutriant is crossed to activated carbon column, collect liquid, obtain chlorogenic acid.
Preferably, described step a is that after Japanese Honeysuckle is pulverized, to add volume fraction be 60% ~ 80% ethanol, and pH is adjusted to 3 ~ 5, soaks 24-72 hour, then broken wall lixiviate.
Preferred, described step a is that after Japanese Honeysuckle is pulverized, to add volume fraction be 70% ethanol, and pH is adjusted to 4, soaks then broken wall lixiviate 24 hours.
Preferred, described broken wall lixiviate is under 50 DEG C ~ 70 DEG C conditions, and ultrasonic extraction twice each 30 minutes, merges extracted twice liquid.
Preferred, described broken wall lixiviate is to process 1 ~ 3 minute under output rating is the microwave condition of 600 W, is to extract twice under 70-90 DEG C of condition with ethanol in temperature, 90 minutes for the first time, 30 minutes for the second time, merges extracted twice liquid.
Preferably, described step a replaces by following steps: after Japanese Honeysuckle is pulverized, add water, soak 24-72 hour, then add the polygalacturonase that is equivalent to Japanese Honeysuckle weight 0.2% ~ 0.3%, be equivalent to the cellulase of Japanese Honeysuckle weight 0.5% ~ 0.6%, enzymolysis 2.5 hours under 35 DEG C ~ 45 DEG C conditions is then used twice of extraction using alcohol under 80 DEG C of conditions, each 2 hours, merge extracted twice liquid.
Preferably, step a gained crude extract is concentrated into medicinal extract by described step b, adds and be equivalent to 5-15 times of water dissolution of medicinal extract volume.
Preferably, described step c adds supernatant liquor in resin absorbing column, after rinsing with the water of 5-10 times of column volume, wash post with the ethanolic soln that the volume fraction of 5-10 times of column volume is 10% ~ 50% again, collect elutriant, elutriant anhydrous alcohol solution, supernatant liquor is crossed to activated carbon column, collect liquid.
Beneficial effect of the present invention: the invention provides the method for chlorogenic acid extracting from Japanese Honeysuckle, its technique is simple, and extraction cost is low, in leaching process pulverizes Japanese Honeysuckle, has increased the surface-area extracting, and is conducive to abundant extraction, improves the rate of recovery.In leaching process, adopt ultrasonic extraction, Microwave-Assisted Ethanol extraction method and enzymolysis Assisted Ethanol extraction method, cytoclasis is abundant, ensure extraction efficiency, in order to obtain highly purified chlorogenic acid, extract is first crossed to resin column, refine with charcoal absorption, the chlorogenic acid purity making is high, is up to 85.2% again.
Embodiment
Below in conjunction with specific embodiment, such scheme is described further.Should be understood that these embodiment are not limited to limit the scope of the invention for the present invention is described.The implementation condition adopting in embodiment can be done further adjustment according to the condition of concrete producer, and not marked implementation condition is generally the condition in normal experiment.
embodiment 1
The method of chlorogenic acid extracting, comprises the steps:
A. after Japanese Honeysuckle being pulverized, adding volume fraction is 60% ethanol, and feed liquid weight ratio is 1:10, and pH is adjusted to 3, soaks 72 hours, and then under 50 DEG C of conditions, ultrasonic extraction twice, each 30 minutes, merging extracted twice liquid, made crude extract;
B. step a gained crude extract is concentrated into medicinal extract, adds the water dissolution that is equivalent to 10 times of medicinal extract weight, get supernatant liquor; Repeat 3 times, merge supernatant liquor, concentrated;
C. step b gained concentrated solution is added to (the preferred HPD100 model of adsorption column macroporous resin column) in resin absorbing column, after rinsing with 5 times of cylinder ponding, wash post with the ethanolic soln that the volume fraction of 5 times of column volumes is 10% again, collect elutriant, elutriant is crossed to activated carbon column, collect elutriant, obtain chlorogenic acid.
In the present embodiment, the rate of recovery of chlorogenic acid is 18.2%, and purity is 61.0%.
embodiment 2
The method of chlorogenic acid extracting, comprises the steps:
A. after Japanese Honeysuckle being pulverized, adding volume fraction is 80% ethanol, and feed liquid weight ratio is 1:20, and pH is adjusted to 4, soaks 36 hours, and then under 70 DEG C of conditions, ultrasonic extraction twice, each 30 minutes, merging extracted twice liquid, made crude extract;
B. step a gained crude extract is concentrated into medicinal extract, adds the water dissolution that is equivalent to 5 times of medicinal extract weight, get supernatant liquor; Repeat 3 times, merge supernatant liquor, concentrated;
C. concentrated solution on step b gained is added to (the preferred HPD100 model of adsorption column macroporous resin column) in resin absorbing column, after rinsing with 5 times of cylinder ponding, wash post with the ethanolic soln that the volume fraction of 5 times of column volumes is 10% again, collect elutriant, elutriant is crossed to activated carbon column, collect elutriant, obtain chlorogenic acid.
In the present embodiment, the rate of recovery of chlorogenic acid is 21.4%, and purity is 62.5%.
embodiment 3
The method of chlorogenic acid extracting, comprises the steps:
A. after Japanese Honeysuckle being pulverized, adding volume fraction is 60% ethanol, feed liquid weight ratio is 1:15, and pH is adjusted to 3, soaks 72 hours, be to process 3 minutes under the microwave condition of 600 W in output rating, be to extract twice under 70 DEG C of conditions with ethanol in temperature, 90 minutes for the first time, 30 minutes for the second time, merge extracted twice liquid, make crude extract;
B. step a gained crude extract is concentrated into medicinal extract, adds the water dissolution that is equivalent to 15 times of medicinal extract weight, get supernatant liquor; Repeat 3 times, merge supernatant liquor, concentrated;
C. concentrated solution on step b gained is added to (the preferred HPD100 model of adsorption column macroporous resin column) in resin absorbing column, after rinsing with 8 times of cylinder ponding, wash post with the ethanolic soln that the volume fraction of 8 times of column volumes is 20% again, collect elutriant, elutriant is crossed to activated carbon column, collect elutriant, obtain chlorogenic acid.
In the present embodiment, the rate of recovery of chlorogenic acid is 29.1%, and purity is 70.6%.
embodiment 4
The method of chlorogenic acid extracting, comprises the steps:
A. after Japanese Honeysuckle being pulverized, add water, feed liquid weight ratio is 1:20, and pH is adjusted to 4, soaks 36 hours, be to process 1 minute under the microwave condition of 600 W in output rating, be to extract twice under 90 DEG C of conditions with ethanol in temperature, 90 minutes for the first time, 30 minutes for the second time, merge extracted twice liquid, make crude extract;
B. step a gained crude extract is concentrated into medicinal extract, adds the water dissolution that is equivalent to 5 times of medicinal extract weight, get supernatant liquor; Repeat 3 times, merge supernatant liquor, concentrated;
C. concentrated solution on step b gained is added to (the preferred HPD100 model of adsorption column macroporous resin column) in resin absorbing column, after rinsing with 8 times of cylinder ponding, wash post with the ethanolic soln that the volume fraction of 8 times of column volumes is 50% again, collect elutriant, elutriant is crossed to activated carbon column, collect elutriant, obtain chlorogenic acid.
In the present embodiment, the rate of recovery of chlorogenic acid is 31.9%, and purity is 72.6%.
embodiment 5
The method of chlorogenic acid extracting, comprises the steps:
A. after Japanese Honeysuckle being pulverized, add water, feed liquid weight ratio is 1:10, soak 72 hours, then add the polygalacturonase that is equivalent to Japanese Honeysuckle weight 0.2% and the cellulase that is equivalent to Japanese Honeysuckle weight 0.6%, enzymolysis 2.5 hours under 40 DEG C of conditions, then under 80 DEG C of conditions, use twice of extraction using alcohol, each 2 hours, merge extracted twice liquid, make crude extract;
B. step a gained crude extract is concentrated into medicinal extract, adds the water dissolution that is equivalent to 10 times of medicinal extract weight, get supernatant liquor; Repeat 3 times, merge supernatant liquor, concentrated;
C. concentrated solution on step b gained is added to (the preferred HPD100 model of adsorption column macroporous resin column) in resin absorbing column, after rinsing with 5 times of cylinder ponding, wash post with the ethanolic soln that the volume fraction of 5 times of column volumes is 20% again, collect elutriant, elutriant is crossed to activated carbon column, collect liquid, obtain chlorogenic acid.
In the present embodiment, the rate of recovery of chlorogenic acid is 34.6%, and purity is 78.0%.
embodiment 6
The method of chlorogenic acid extracting, comprises the steps:
A. after Japanese Honeysuckle being pulverized, adding volume fraction is 80% ethanol, feed liquid weight ratio is 1:15, soak 36 hours, then add the polygalacturonase that is equivalent to Japanese Honeysuckle weight 0.3% and the cellulase that is equivalent to Japanese Honeysuckle weight 0.5%, enzymolysis 2.5 hours under 45 DEG C of conditions, then under 80 DEG C of conditions, use twice of extraction using alcohol, each 2 hours, merge extracted twice liquid, make crude extract;
B. step a gained crude extract is concentrated into medicinal extract, adds the water dissolution that is equivalent to 15 times of medicinal extract weight, get supernatant liquor; Repeat 3 times, merge supernatant liquor, concentrated;
C. concentrated solution on step b gained is added to (the preferred HPD100 model of adsorption column macroporous resin column) in resin absorbing column, after rinsing with 5 times of cylinder ponding, wash post with the ethanolic soln that the volume fraction of 5 times of column volumes is 20% again, collect elutriant, elutriant is crossed to activated carbon column, collect liquid, obtain chlorogenic acid.
The present embodiment is most preferred embodiment of the present invention, and the rate of recovery of chlorogenic acid is 38.4%, and purity is 85.2%.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although by with reference to the preferred embodiments of the present invention, invention has been described, but those of ordinary skill in the art is to be understood that, can make various changes to it in the form and details, and not depart from the present invention that appended claims limits.
Claims (2)
1. the method for chlorogenic acid extracting, is characterized in that, extraction step is as follows:
A. after Japanese Honeysuckle being pulverized, adding volume fraction is 60% ~ 80% ethanol, and feed liquid weight ratio is 1:10-20, and pH is adjusted to 3 ~ 5, soaks 24-72 hour, and then broken wall lixiviate, makes crude extract; Described broken wall lixiviate is under 50 DEG C ~ 70 DEG C conditions, and ultrasonic extraction twice each 30 minutes, merges extracted twice liquid;
B. step a gained crude extract is concentrated into medicinal extract, adds water and be equivalent to 5-15 times of water dissolution of medicinal extract volume, get supernatant liquor;
C. supernatant liquor is added in resin absorbing column, after rinsing, then wash post with the ethanolic soln that the volume fraction of 5-10 times of column volume is 20% with the water of 5-10 times of column volume, collect elutriant, elutriant anhydrous alcohol solution, crosses activated carbon column by supernatant liquor, collects liquid.
2. the method for chlorogenic acid extracting according to claim 1, is characterized in that: described step a is that after Japanese Honeysuckle is pulverized, to add volume fraction be 70% ethanol, and feed liquid weight ratio is 1:15, and pH is adjusted to 4, soaks then broken wall lixiviate 24 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210453316.7A CN102911055B (en) | 2012-11-13 | 2012-11-13 | Method for extracting chlorogenic acid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210453316.7A CN102911055B (en) | 2012-11-13 | 2012-11-13 | Method for extracting chlorogenic acid |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102911055A CN102911055A (en) | 2013-02-06 |
| CN102911055B true CN102911055B (en) | 2014-07-09 |
Family
ID=47609661
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210453316.7A Expired - Fee Related CN102911055B (en) | 2012-11-13 | 2012-11-13 | Method for extracting chlorogenic acid |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102911055B (en) |
Families Citing this family (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103086889B (en) * | 2013-02-22 | 2015-11-25 | 王星敏 | A kind of method of enzyme catalysis activation leaf of Flos Lonicerae chlorogenic acid extracting |
| CN103787885B (en) * | 2014-03-06 | 2016-08-24 | 山东禾本堂生物科技有限公司 | A kind of method extracting high-purity chlorogenic acid from Flos Lonicerae aerial parts |
| CN104788314A (en) * | 2015-04-03 | 2015-07-22 | 广西大学 | Method for extracting chlorogenic acid from honeysuckle flowers |
| CN105085257B (en) * | 2015-06-24 | 2017-11-03 | 四川农业大学 | A kind of method that weight chlorogenic acid is extracted from Eupatorium adenophorum |
| CN106071622B (en) * | 2016-06-15 | 2020-03-20 | 河北省农林科学院经济作物研究所 | Clear honeysuckle solid beverage and preparation method thereof |
| CN108586241B (en) * | 2018-01-17 | 2021-03-05 | 浙江树人学院 | Method for extracting and separating chlorogenic acid of sweet potato leaves by ultrasonic-microwave-aqueous two-phase cooperation |
| CN108653370A (en) * | 2018-07-31 | 2018-10-16 | 庐山市环绿时代农业科技开发有限公司 | A kind of preparation method of honeysuckle particle |
| CN109809997A (en) * | 2019-03-07 | 2019-05-28 | 四川君正生物饲料有限公司 | A method of the chlorogenic acid extracting from coffee grounds |
| CN110305007A (en) * | 2019-07-25 | 2019-10-08 | 广西民族大学 | One kind extracting caffeinic method from a silk fabric |
| CN111153759A (en) * | 2020-01-17 | 2020-05-15 | 金陵药业股份有限公司 | Method for extracting total phenolic acid from waste liquid of ester extraction in Mailuoning injection production |
| CN113875844A (en) * | 2021-09-29 | 2022-01-04 | 武夷山成隆天创茶业科技股份有限公司 | Application of spartina alterniflora extract in plant-derived functional tea product and functional tea product |
| CN114031498A (en) * | 2021-11-05 | 2022-02-11 | 临沂市农业科学院 | Method for extracting high-purity honeysuckle chlorogenic acid by membrane separation method |
| CN114751825A (en) * | 2022-05-24 | 2022-07-15 | 河北瑞龙生物科技有限公司 | Method for efficiently extracting chlorogenic acid from honeysuckle |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314568A (en) * | 2008-06-24 | 2008-12-03 | 南京工业大学 | Novel method for adsorption separation of high purity chlorogenic acid |
| CN101830804A (en) * | 2010-03-16 | 2010-09-15 | 天津中新药业集团股份有限公司中新制药厂 | Method for extracting chlorogenic acid from honeysuckle by using compound enzyme method |
| CN101838200A (en) * | 2009-03-20 | 2010-09-22 | 上海中医药大学 | Method for extracting and separating chlorogenic acid from honeysuckle |
| CN102476996A (en) * | 2010-11-22 | 2012-05-30 | 郭翀 | Extraction process of chlorogenic acid in honeysuckle |
-
2012
- 2012-11-13 CN CN201210453316.7A patent/CN102911055B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101314568A (en) * | 2008-06-24 | 2008-12-03 | 南京工业大学 | Novel method for adsorption separation of high purity chlorogenic acid |
| CN101838200A (en) * | 2009-03-20 | 2010-09-22 | 上海中医药大学 | Method for extracting and separating chlorogenic acid from honeysuckle |
| CN101830804A (en) * | 2010-03-16 | 2010-09-15 | 天津中新药业集团股份有限公司中新制药厂 | Method for extracting chlorogenic acid from honeysuckle by using compound enzyme method |
| CN102476996A (en) * | 2010-11-22 | 2012-05-30 | 郭翀 | Extraction process of chlorogenic acid in honeysuckle |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102911055A (en) | 2013-02-06 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102911055B (en) | Method for extracting chlorogenic acid | |
| CN102491938B (en) | A kind of purification process of S-GI | |
| CN102219824B (en) | Method for producing glycyrrhizic acid through enzymolysis | |
| CN102701914B (en) | Method for extracting hydroxytyrosol from olive leaves | |
| CN103694364A (en) | Method for synchronously extracting, separating and purifying polysaccharides and flavones of cyclocarya paliurus | |
| CN102276424B (en) | Method for preparing hydroxytyrosol by boiling and hydrolyzing | |
| CN101775056A (en) | Method for extracting, separating and purifying Astragaloside IV from Astragalus mongholicus | |
| CN103467617A (en) | Method for continuous counter-current ultrasonic extraction of high-purity astragalus polysaccharide | |
| CN101775418A (en) | Method for extracting, separating and purifying formononetin and calycosin from Astragalus mongholicus waste residue | |
| CN102432535A (en) | Method for extracting and separating huperzine A and huperzine B from huperzia serrata | |
| CN103304576A (en) | Method for extracting artemisinin through enzymatic hydrolysis | |
| CN105753917B (en) | A kind of isolation and purification method of liquiritin | |
| CN102716208A (en) | Preparation method for general flavone extract from seed coats of peony | |
| WO2012068832A1 (en) | Method for preparing mogroside iv | |
| CN104073361A (en) | Method for extracting artemisia apiacea volatile oil | |
| CN102204950B (en) | Method for extracting flavonoid from liquorice waste residue | |
| CN102702101B (en) | A kind of method extracting selagine from Herba Lycopodii serrati | |
| CN104263763A (en) | Novel method for extracting resveratrol from giant knotweed | |
| CN107519232A (en) | One kind extraction Gueldenstaedtia verna extractive of general flavone and preparation method thereof | |
| CN103641716A (en) | Method for extracting refined chicoric acid | |
| CN103305564A (en) | Method for converting icariin to herba epimedii | |
| CN105294793A (en) | Separation method for naringin in aizoon stonecrop herb | |
| CN105111144A (en) | Method of extracting nuciferine from lotus leaves | |
| CN110141605A (en) | A kind of preparation method of snowpoppy total alkaloid nanoparticle | |
| CN107723315A (en) | A kind of new method for separating giant knotweed composition and preparing resveratrol |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20140709 Termination date: 20161113 |