CN101367729B - Method for complexation purification by liquid extraction of chlorogenic acid - Google Patents
Method for complexation purification by liquid extraction of chlorogenic acid Download PDFInfo
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Abstract
The present invention relates to a method of purifying chlorogenic acid with the complexation extraction technology. A complexation extractant used as a light phase for extraction contacts with plant extract used as a heavy phase to perform complexation and extraction; and the organic phase with the chlorogenic acid is stripped to prepare high-purity chlorogenic acid. The present invention is suitable of low-concentration plant extract; when the separation process of complexing and extracting the chlorogenic acid is used, the production cost can be decreased, the organic solvent residue can be reduced, the environmental pollution is slowed, and the present invention fits requirements of the green chemical technology.
Description
Technical field
The present invention relates to a kind of method of complexation purification by liquid extraction of chlorogenic acid, belong to natural product purification field.
Background technology
Chlorogenic acid is a kind of polyphenolic compound, it is the class biologically active substance that occurring in nature extensively exists, mainly being distributed in the plants such as Caprifoliaceae, the Rosaceae, composite family, Rubiaceae and Eucommiaceae, is that traditional Chinese medicines such as the bark of eucommia, Japanese Honeysuckle are clearing heat and detoxicating, the main component of antiphlogistic antibacterial.Studies show that that chlorogenic acid has is antibiotic, antiviral, anti-oxidant, remove free radical, immunomodulatory, pharmacological action such as antitumor, anti-lipid.Therefore, the application of chlorogenic acid in biochemical reagents, pharmaceutical intermediate and formulation art is internationally recognized at present " plant gold " more and more widely.Because chlorogenic acid often is present in nature jointly with its isomer or analogue, mutual physico-chemical property difference is less, the separation and purification difficulty of chlorogenic acid is big for a long time, cost is high, so the research of the preparation of high-purity chlorogenic acid and separation purifying technique thereof is one of focus of current natural product research.
The producer that produces pharmaceutical or biochemical level chlorogenic acid at present is considerably less, and high-purity chlorogenic acid yields poorly, involves great expense, and can not satisfy the market requirement both domestic and external far away.In the process of preparation high-purity chlorogenic acid, the chlorogenic acid loss is very serious, falls behind and prepare chlorogenic acid crude extract technology at present, lacks the efficient purification techniques that satisfies the scale operation needs.China's chlorogenic acid aboundresources is planted and is implanted with multiple plant of being rich in chlorogenic acid, and as Japanese Honeysuckle, the bark of eucommia, coffee berry, tobacco, oriental wormwood, sunflower seeds, Herba Arctii leaf and Acer Truncatum Buge leaf etc., exploitation chlorogenic acid related products has high economic worth and market outlook.U.S. Pat 4872987, German patent DE 3603574 and DE3239219, European patent EP 1405566, International Patent Application WO 2006093114 and WO2006080333, Japanese Patent JP4145049, JP4145048, JP2005263632, JP2006174746, the technical scheme of disclosed preparation high-purity chlorogenic acid such as JP2007031392 and JP2007322823 all is on the basis of slightly carrying, further adopt modern separation means, separate as absorption with macroporous adsorbent resin, ion exchange column separates, it is refining that polymeric amide or sephadex chromatography method etc. are carried out further chlorogenic acid; Chinese patent CN1398845, CN1762972, CN1616403, CN1687008, CN1524843, the disclosed chlorogenic acid process for purification of CN1435406 all adopts column chromatography for separation, related adsorption stuffing comprises macroporous adsorbent resin, ion exchange resin and polymeric amide, in view of the easy oxidation of chlorogenic acid institute phenolic hydroxy group, olefin(e) acid ester bond facile hydrolysis and intramolecularly ester group be the characteristic of migration easily, though chromatography can prepare the chlorogenic acid of higher degree, but can not realize high efficiency separation, chlorogenic acid oxidation and isomery make productive rate descend, and this method cost is higher, and production intensity is limited; Chinese patent CN1616402, CN1746149, CN1740137, CN1425643, the disclosed chlorogenic acid process for purification of CN1273964 and CN1273964 is solvent extraction and column chromatography coupling, promptly utilize solvent extraction to obtain utilizing column chromatography refining behind the crude product earlier, this method can obtain the chlorogenic acid of higher degree, but used extraction agent ethyl acetate is water-soluble big in the solvent extraction process, residual height in water, influence the chlorogenic acid product purity, increase water pollution degree, and this method steps is loaded down with trivial details, the solvent recuperation power consumption is serious, the production cost height is unsuitable for industry and amplifies; Chinese patent CN1810763 discloses a kind of membrane sepn and supercritical CO
2The method of the refining chlorogenic acid of extraction coupling, but this method only is fit to prepared in laboratory, also can't realize the industry amplification at present.
Early 1980s, professor C.J.King of California, USA university has proposed a kind of polar organic matter extraction separating method based on reversible complex reaction, abbreviates complexing abstraction as.In this class technological process, solute to be separated contacts with the extraction solvent that contains complexing agent in the solution, and complexing agent and solute reacting forming complex to be separated are transferred in the extraction phase it, and finished the reextraction process by hunt effect, realizes separating purpose.Compare with the method for the exquisite chlorogenic acid of using always at present, complexing abstraction has the separation efficiency height, throughput is big, and energy consumption is low, pollutes little, be convenient to rapidly, continuously advantages such as operation with safety, gained chlorogenic acid purity is higher than simple extracting and separating gained far away, and throughput is also far above column chromatography, and the complexing extractant reusable edible, reduce production cost greatly, disclosed a kind of method of acidic extractant complexing extraction separation rare-earth element as Chinese patent CN101182597.So far, do not utilize method that complexing abstraction separates chlorogenic acid at home, do not appear in the newspapers as yet outward.
Summary of the invention
Technical purpose of the present invention is the weak point at existing chlorogenic acid purification techniques, a kind of novel method of complexation purification by liquid extraction of chlorogenic acid is provided, make this method go for the lower concentration plant extraction liquid, complexometric extraction chlorogenic acid separating technology can reduce production costs, reduce organic solvent residual, alleviate the pollution of environment, meet the requirement of green chemistry process.
In order to realize technical purpose of the present invention, the present invention proposes following technical scheme:
A kind of method of complexation purification by liquid extraction of chlorogenic acid, it is characterized in that contacting with plant extraction liquid as the light of extracting and separating as heavy phase with complexing extractant, finish the complex reaction extraction process, the gained collection has the organic phase of chlorogenic acid to obtain high-purity chlorogenic acid through reextraction.
Concrete steps comprise:
(1) preparation complexing extractant
Complexing agent, solubility promoter and thinner are mixed with complexing extractant, or complexing agent and thinner are mixed with complexing extractant mutually light as extracting and separating;
(2) complex reaction extraction
Regulate the heavy phase of pH value to 1～5 of plant extraction liquid, mix with light volume ratio and carry out complex reaction and mass transfer with 5:1～15:1 as extracting and separating, 5～25 ℃ of control extraction temperature, standing demix obtains coming together the upper organic phase of chlorogenic acid;
(3) strip
After upper organic phase pH is the washing of 1～5 acid solution, with pH is that 5～12 acid solution or alkaline solution are as the heavy phase of stripping, carry out decomplexing with the organic light volume ratio mixing in upper strata and close reaction and mass transfer with 5:1～20:1, the reextraction temperature is 25～65 ℃, the extraction agent after obtaining the pure solution of chlorogenic acid after the static layering and regenerating.
The pure solution of gained chlorogenic acid of the present invention can drying obtain the chlorogenic acid powder so that reprocess, transport or preserve through regulating pH to 1～5 rapidly with anti-oxidation.
Plant extraction liquid of the present invention comprises the aqueous extract after the de-oiling of Japanese Honeysuckle, the bark of eucommia, coffee berry, tobacco or discarded tobacco shred, oriental wormwood, sunflower seeds, Herba Arctii leaf or Acer Truncatum Buge leaf.
The concentration range of chlorogenic acid is 0.5～20g/L in the plant extraction liquid of the present invention.
Complexing agent of the present invention comprises tributyl phosphate, trioctyl phosphate, trioctylphosphine oxide (TOPO) or trialkylphosphine oxide.
Solubility promoter of the present invention comprises butylacetate, methyl iso-butyl ketone (MIBK), n-Octanol, primary isoamyl alcohol or n-hexyl alcohol.
Thinner of the present invention comprises tasteless kerosene, aviation kerosene, diesel oil or normal paraffin C
8～C
12
The concentration of complexing agent is 5%～40% in the complexing extractant of the present invention.
The ratio of solubility promoter of the present invention and thinner is 0～1:8.
The acid solution of adjusting pH value of the present invention and reextraction usefulness comprises hydrochloric acid, sulfuric acid or acetic acid.
The alkaline solution of adjusting pH value of the present invention and reextraction usefulness comprises sodium hydroxide, potassium hydroxide, yellow soda ash or sodium bicarbonate.
Beneficial effect of the present invention is:
(1) adopt complexometric extraction to prepare the method for chlorogenic acid: this extraction process is simply efficient, and the extraction conditions gentleness has effectively reduced the degree of decomposition of chlorogenic acid, thereby has improved the purity and the yield of chlorogenic acid; And used complexing agent, solubility promoter and thinner is water-soluble all less, and extraction back water Determination of Residual Organic Solvents is low; The reextraction process is the complexing extractant regenerative process, need not carry out the complexing extractant regenerative operation in addition, therefore operation energy consumption is low, and complexing extractant can be recycled, discharge amount of pollution is low, production cost can not improve because of the use of complexing agent, helps the control and the management of production process more, is a kind of good Green Chemistry extraction separation process;
(2) solubility promoters such as butylacetate are adopted in selection: this extraction process has selected for use butylacetate, methyl iso-butyl ketone (MIBK), n-Octanol, primary isoamyl alcohol or n-hexyl alcohol as solubility promoter, reduced the emulsification effect of complexing agent, and selected solubility promoter is water-soluble all less, is difficult for producing organic residual.Separation factor through between extraction gained chlorogenic acid and impurity is between 95～300, is higher than the separation factor (12～28) of simple organic solvent extraction far away;
(3) adopted the method for regulating the pH value of plant extraction liquid: chlorogenic acid exists with molecular form in pH1～5 scopes, be difficult for oxidation and isomery, and be easy to also can enter fast in the organic phase with complexing agent generation complex reaction, and the difficult and complexing agent generation complex reaction of impurity in the aqueous extract in this pH value scope, increase the separation factor between chlorogenic acid and the impurity, thereby effectively improved the purity of chlorogenic acid;
(4) method of employing low-temperature extraction: the complex reaction that is taken place during owing to complexing extractant extraction chlorogenic acid belongs to thermopositive reaction, adopt low-temperature extraction can exchange the heat that complex reaction produces effectively, accelerate complexing agent and chlorogenic acid complex reaction speed, thereby improve extraction rate effectively, make the easier organic phase that enters of chlorogenic acid;
(5) adopted the reextraction method of temperature and pH coupling: by regulating strip liquor pH to 5～12, make in the organic phase chlorogenic acid complex compound separate the complexing reaction, and by regulating back extraction temperature to 25～65 ℃, that accelerates the chlorogenic acid complex compound separates complexing speed of reaction and reextraction speed, thereby realize the efficient reextraction of chlorogenic acid, and finish the regeneration and the recycling of complexing extractant, and reduced the consumption of organic solvent, saved production cost.
Embodiment:
Among the embodiment of the present invention, chlorogenic acid adopts reversed-phased high performace liquid chromatographic to detect, and used chromatographic column is Alltima C
18(150mm * 4.6mm), used moving phase be ammonium acetate buffer-acetonitrile (95:5, V/V), detecting wavelength is 327nm, flow velocity is 1mL/min.
Flavonoid substances adopts reversed-phased high performace liquid chromatographic to detect, and used chromatographic column is Alltima C
18(150mm * 4.6mm), used moving phase be pH4.5 aqueous acetic acid-methyl alcohol (50:50, V/V), detecting wavelength is 360nm, flow velocity is 1mL/min.
Separation factor is according to the partition ratio D of experiment gained chlorogenic acid and impurity, by separation factor β=D
Chlorogenic acid/ D
ImpurityCalculating can get.
Embodiment 1
Adopt that aqueous extract is a raw material after the Japanese Honeysuckle de-oiling that the pH value is 2, chlorogenic acid concentration is 0.5g/L, tributyl phosphate is a complexing agent, butylacetate is a solubility promoter, aviation kerosene is a thinner, the volume ratio of complexing agent, solubility promoter and thinner is mixed with complexing extractant by 1:1:18, with stock liquid and complexing extractant by volume 5:1 in separating funnel, mix vibration, extraction temperature is 5 ℃, static layering behind the ready to balance, obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 2 aqueous hydrochloric acid washing 3 times with the pH value, with the pH value be 11 aqueous sodium hydroxide solution by volume 1:5 in separating funnel, mix vibration, temperature is 35 ℃, the reextraction number of times is 5 times, merge anti-stripping agent, regulate anti-stripping agent pH to 3 with hydrochloric acid, it is 85.74% that drying under reduced pressure obtains the chlorogenic acid product purity, and yield is 90.88%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 270.
Embodiment 2
Adopt that aqueous extract is a raw material after the Folium Eucommiae de-oiling that the pH value is 1, chlorogenic acid concentration is 20g/L, trioctyl phosphate is a complexing agent, methyl iso-butyl ketone (MIBK) is a solubility promoter, diesel oil is thinner, the volume ratio of complexing agent, solubility promoter and thinner is mixed with complexing extractant by 1:1:15, will stir in stock liquid and the complexing extractant 15:1 adding by volume constant interfacial area cell, and extraction temperature is 25 ℃, static layering behind the ready to balance, obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 1 aqueous hydrochloric acid washing 2 times with the pH value, with the pH value be 8 aqueous sodium carbonate by volume 1:20 add in the constant interfacial area cell and stir, temperature is 65 ℃, the reextraction number of times is 4 times, merge anti-stripping agent, regulate anti-stripping agent pH to 3 with hydrochloric acid, it is 81.37% that lyophilize obtains the chlorogenic acid product, and yield is 88.21%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 198.
Embodiment 3
Adopt that aqueous extract is a raw material after the tobacco de-oiling that the pH value is 5, chlorogenic acid concentration is 5g/L, trialkylphosphine oxide is a complexing agent, tasteless kerosene is a thinner, the volume ratio of complexing agent and thinner is mixed with complexing extractant by 2:5, with stock liquid and complexing extractant by volume the 10:1 adverse current pass through extraction tower, extraction temperature is 15 ℃, static layering behind the ready to balance, and obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 5 aqueous hydrochloric acid washing 6 times with the pH value, with the pH value be 6.5 sodium bicarbonate aqueous solution by volume 1:10 add in the constant interfacial area cell and stir, temperature is 25 ℃, the reextraction number of times is 8 times, merge anti-stripping agent, regulate anti-stripping agent pH to 3 with hydrochloric acid, it is 72.73% that spraying drying obtains the chlorogenic acid product purity, and yield is 87.62%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 115.
Embodiment 4
Adopt that aqueous extract is a raw material after the coffee berry de-oiling that the pH value is 2, chlorogenic acid concentration is 20g/L, trialkylphosphine oxide is a complexing agent, n-hexyl alcohol is a solubility promoter, tasteless kerosene is a thinner, the volume ratio of complexing agent, solubility promoter and thinner is mixed with complexing extractant by 2:1:19, will stir in stock liquid and the complexing extractant 1:20 adding by volume constant interfacial area cell, and extraction temperature is 5 ℃, static layering behind the ready to balance, obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 3 aqueous sulfuric acid washing 1 time with the pH value, with the pH value be 12 potassium hydroxide aqueous solution by volume 1:10 add in the constant interfacial area cell and stir, temperature is 45 ℃, the reextraction number of times is 2 times, merge anti-stripping agent, regulate anti-stripping agent pH to 3 with hydrochloric acid, it is 77.54% that drying under reduced pressure obtains the chlorogenic acid product purity, and yield is 84.66%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 300.
Embodiment 5
Adopt that aqueous extract is a raw material after the pipe tobacco waste de-oiling that the pH value is 1, chlorogenic acid concentration is 8g/L, trioctylphosphine oxide (TOPO) is a complexing agent, n-Octanol is a solubility promoter, diesel oil is thinner, with n-Octanol with after the trioctylphosphine oxide (TOPO) dissolving, with thinner by volume 1:10 be mixed with complexing extractant (trioctylphosphine oxide (TOPO) is 15%), with stock liquid and complexing extractant by volume the 5:1 adverse current by the extraction rotating disc contactor, extraction temperature is 10 ℃, static layering behind the ready to balance, obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 5 aqueous acetic acid washing 5 times with the pH value, with the pH value be 5 sulphuric acid soln by volume the 1:15 adverse current by the extraction rotating disc contactor, temperature is 55 ℃, the reextraction number of times is 6 times, merge anti-stripping agent, regulate anti-stripping agent pH to 3 with sulfuric acid, it is 73.82% that lyophilize obtains the chlorogenic acid product purity, and yield is 91.51%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 95.
Embodiment 6
Adopt that aqueous extract is a raw material after the oriental wormwood de-oiling that the pH value is 5, chlorogenic acid concentration is 7.5g/L, trioctyl phosphate is a complexing agent, and primary isoamyl alcohol is a solubility promoter, normal paraffin C
8～C
12Be thinner, the volume ratio of complexing agent, solubility promoter and thinner is mixed with complexing extractant by 1:1:10, with stock liquid and complexing extractant by volume 10:1 in separating funnel, mix vibration, extraction temperature is 20 ℃, static layering behind the ready to balance, obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 3 aqueous acetic acid washing 2 times with the pH value, with the pH value be 8 sodium bicarbonate aqueous solution by volume 1:10 in separating funnel, mix vibration, temperature is 25 ℃, the reextraction number of times is 5 times, merge anti-stripping agent, regulate anti-stripping agent pH to 3 with acetic acid, it is 68.53% that spraying drying obtains the chlorogenic acid product purity, and yield is 76.32%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 173.
Embodiment 7
Adopt that aqueous extract is a raw material after the sunflower seeds de-oiling that the pH value is 2, chlorogenic acid concentration is 15g/L, trialkylphosphine oxide is a complexing agent, and butylacetate is a solubility promoter, normal paraffin C
8～C
12Be thinner, the volume ratio of complexing agent, solubility promoter and thinner is mixed with complexing extractant by 2:1:8, and the 8:1 adverse current is by hollow-fibre membrane by volume with stock liquid and complexing extractant, and extraction temperature is 10 ℃, static layering behind the ready to balance, obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 4 aqueous hydrochloric acid washing 4 times with the pH value, with the pH value be 10 potassium hydroxide solution by volume the 1:12 adverse current pass through hollow-fibre membrane, temperature is 65 ℃, the reextraction number of times is 6 times, merge anti-stripping agent, regulate anti-stripping agent pH to 3 with hydrochloric acid, it is 65.61% that drying under reduced pressure obtains the chlorogenic acid product purity, and yield is 90.63%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 148.
Embodiment 8
Adopt that aqueous extract is a raw material after the Herba Arctii leaf de-oiling that the pH value is 3, chlorogenic acid concentration is 2g/L, trioctylphosphine oxide (TOPO) is a complexing agent, n-Octanol is a solubility promoter, tasteless kerosene is a thinner, with n-Octanol with after the trioctylphosphine oxide (TOPO) dissolving, with thinner by volume 1:12 be mixed with complexing extractant (trioctylphosphine oxide (TOPO) is 10%), with stock liquid and complexing extractant by volume the 11:1 adverse current by the extraction rotating disc contactor, extraction temperature is 15 ℃, static layering behind the ready to balance, obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 1 aqueous sulfuric acid washing 5 times with the pH value, with the pH value be 9 sodium bicarbonate aqueous solution by volume the 1:15 adverse current by the extraction rotating disc contactor, temperature is 60 ℃, the reextraction number of times is 8 times, merge anti-stripping agent, regulate anti-stripping agent pH to 2 with sulfuric acid, it is 66.19% that lyophilize obtains the chlorogenic acid product purity, and yield is 89.22%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 274.
Embodiment 9
Adopt that aqueous extract is a raw material after the Acer Truncatum Buge leaf de-oiling that the pH value is 4, chlorogenic acid concentration is 4g/L, tributyl phosphate is a complexing agent, n-hexyl alcohol is a solubility promoter, aviation kerosene is a thinner, the volume ratio of complexing agent, solubility promoter and thinner is mixed with complexing extractant by 2:1:9, and the 15:1 adverse current is by hollow-fibre membrane by volume with stock liquid and complexing extractant, and extraction temperature is 5 ℃, static layering behind the ready to balance, obtaining coming together has the upper organic phase of chlorogenic acid.
After above-mentioned organic phase is 4 aqueous acetic acid washing 3 times with the pH value, with the pH value be 11 potassium hydroxide aqueous solution by volume the 1:20 adverse current pass through hollow-fibre membrane, temperature is 45 ℃, the reextraction number of times is 5 times, merge anti-stripping agent, regulate anti-stripping agent pH to 2.5 with acetic acid, it is 85.37% that spraying drying obtains the chlorogenic acid product purity, and yield is 90.65%.
The body series major impurity is a Flavonoid substances, and according to the partition ratio of above-mentioned experiment gained chlorogenic acid and Flavonoid substances, calculating separation factor is 220.
Claims (3)
1. the method for a complexation purification by liquid extraction of chlorogenic acid is characterized in that concrete steps comprise:
(1) preparation complexing extractant
Complexing agent, solubility promoter and thinner are mixed with complexing extractant, or complexing agent and thinner are mixed with complexing extractant mutually light as extracting and separating; Wherein, described complexing agent comprises tributyl phosphate, trioctyl phosphate, trioctylphosphine oxide (TOPO) or trialkylphosphine oxide; Described solubility promoter comprises butylacetate, methyl iso-butyl ketone (MIBK), n-Octanol, primary isoamyl alcohol or n-hexyl alcohol; Described thinner comprises tasteless kerosene, aviation kerosene, diesel oil or normal paraffin C
8～C
12
(2) complex reaction extraction
Get the plant extraction liquid that the chlorogenic acid concentration range is 0.5～20g/L, regulate the heavy phase of its pH value to 1～5 as extracting and separating, carry out complex reaction and mass transfer with light volume ratio mixing with 5: 1～15: 1,5～25 ℃ of control extraction temperature, standing demix obtains coming together the upper organic phase of chlorogenic acid; Wherein, described plant extraction liquid comprises the aqueous extract after the de-oiling of Japanese Honeysuckle, the bark of eucommia, coffee berry, tobacco, discarded tobacco shred, oriental wormwood, sunflower seeds, Herba Arctii leaf or Acer Truncatum Buge leaf;
(3) strip
After upper organic phase pH is the washing of 1～5 acid solution, with pH is that 5～12 acid solution or alkaline solution are as the heavy phase of stripping, carry out decomplexing with the organic light volume ratio mixing in upper strata and close reaction and mass transfer with 5: 1～20: 1, the reextraction temperature is 25～65 ℃, the extraction agent after obtaining the pure solution of chlorogenic acid after the static layering and regenerating; Wherein said acid solution comprises hydrochloric acid, sulfuric acid or acetum; Described alkaline solution comprises sodium hydroxide, potassium hydroxide, yellow soda ash or sodium hydrogen carbonate solution.
2. the method for a kind of complexation purification by liquid extraction of chlorogenic acid according to claim 1, the concentration that it is characterized in that complexing agent in the described complexing extractant is 5%～40%.
3. the method for a kind of complexation purification by liquid extraction of chlorogenic acid according to claim 1, the ratio that it is characterized in that described solubility promoter and thinner is 0～1: 8.
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| CN101503356B (en) * | 2009-03-25 | 2013-03-13 | 南京工业大学 | Novel method for preparing high-purity chlorogenic acid |
| CN102241580A (en) * | 2011-01-07 | 2011-11-16 | 长春工业大学 | Method for recovering organic carboxylic acids from corn chemical alcohol reaction kettle residues by utilizing complex extraction |
| CN103360258A (en) * | 2013-08-08 | 2013-10-23 | 内蒙古鑫吉利生物科技有限公司 | Method for extracting chlorogenic acid from coffee beans |
| CN104447331A (en) * | 2014-11-11 | 2015-03-25 | 常州大学 | Method for extracting chlorogenic acid in artemisia scoparia |
| CN105384632B (en) * | 2015-10-19 | 2017-06-16 | 新疆大学 | A kind of preparation method and applications of chlorogenic acid of sunflower seed dregs |
| CN106723289A (en) * | 2017-03-31 | 2017-05-31 | 江苏中烟工业有限责任公司 | A kind of method for lifting papermaking-method reconstituted tobaccos recovery rate |
| CN109502676B (en) * | 2017-09-14 | 2020-09-01 | 中国科学院过程工程研究所 | Method for reducing dosage of extracting agent and reducing content of organic matters in water phase from source of acidic extraction system |
| CN112755586A (en) * | 2020-12-29 | 2021-05-07 | 西安元创化工科技股份有限公司 | Method for extracting phenolic compounds from low-temperature coal tar |
| CN113429288A (en) * | 2021-06-03 | 2021-09-24 | 徐州工程学院 | Method for simultaneously extracting burdock leaf essential oil and chlorogenic acid and application |
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| CN1793105A (en) * | 2005-12-16 | 2006-06-28 | 抚州苍源药业开发有限公司 | Tech. for extracting high purity chlorogenic acid from honeysuckle |
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| CN1793105A (en) * | 2005-12-16 | 2006-06-28 | 抚州苍源药业开发有限公司 | Tech. for extracting high purity chlorogenic acid from honeysuckle |
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| 刘军海等.绿原酸及其提取纯化和应用前景.《粮食与油脂》.2003,(第9期),44-46. * |
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