CN104844584A - Method for extracting puerarin from residue of radix puerariae - Google Patents

Method for extracting puerarin from residue of radix puerariae Download PDF

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Publication number
CN104844584A
CN104844584A CN201510183759.2A CN201510183759A CN104844584A CN 104844584 A CN104844584 A CN 104844584A CN 201510183759 A CN201510183759 A CN 201510183759A CN 104844584 A CN104844584 A CN 104844584A
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puerarin
pueraria lobota
extract
lobota slag
extraction
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CN201510183759.2A
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CN104844584B (en
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朱德艳
王学民
王劲松
徐艳
张婷
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Jingchu University of Technology
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Jingchu University of Technology
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07D—HETEROCYCLIC COMPOUNDS
    • C07D407/00—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00
    • C07D407/02—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings
    • C07D407/04—Heterocyclic compounds containing two or more hetero rings, at least one ring having oxygen atoms as the only ring hetero atoms, not provided for by group C07D405/00 containing two hetero rings directly linked by a ring-member-to-ring-member bond
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/10—Process efficiency
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids

Abstract

The invention discloses a method for extracting puerarin from residue of radix puerariae, which comprises the following steps: extracting kudzuvine root starch to obtain slag and drying, performing ultramicro crushing to obtain the particles with diameter being 1-20 micrometers; mixing the crushed residue of radix puerariae and ethanol, adding beta-cyclodextrin and performing ultrasonic extraction; performing heating reflux, performing pumping filtration for extracting puerarin; performing rotary evaporation on a filtrate to a stiff paste, simultaneously recovering ethanol, drying the obtained extract under vacuum; and performing supercritical carbon dioxide extraction on the extract to obtain the puerarin. According to the invention, beta-cyclodextrin can increase the puerarin solubility and dissolution speed from the root of kudzu vine. The method for performing supersonic wave extraction, separating and purifying puerarin has the advantages of short production period, high efficiency, simple equipment, little boiler heat supply and cooling water, saved energy consumption, reduced environment pollution, and low product cost. A used extractant (CO2) is gas which is easily removed, the obtained product has no residual toxicity, and is especially suitable for medicine and food industries.

Description

The method of puerarin is extracted in a kind of Pueraria lobota slag
Technical field
The invention belongs to technical field of extraction of Chinese traditional medicine, be specifically related to a kind of method extracting puerarin in Pueraria lobota slag.
Background technology
The root of kudzu vine (Radix puerariae) is the dry root of legume pueraria lobata Pueraria lobata (Willd.) Ohwi or sweet kudzu Puerariathomsonii Benth.Puerarin is distinctive composition in the root of kudzu vine, also be principle active component, platelet aggregation can be suppressed, reduce the pharmacological actions such as blood sugar, also be the medicinal herbs most in use of control cardiovascular and cerebrovascular diseases, the effect of relieving the effect of alcohol in addition in daily life, has the good reputation of ginseng in thousand, therefore, the root of kudzu vine is widely used in functional food and biological medicine.Current root of kudzu vine processing extractive technique remains in many imperfection parts, particularly be only limitted to extract kudzuvine root starch to the major part that utilizes of Pueraria lobota, and discarded very important medicinal effective active composition flavonoid, and topmost activeconstituents puerarin rare product in the market especially in flavones ingredient, the extraction of puerarin has also become one of study hotspot, but also there are some defects in current many methods, such as many methods employ a large amount of organic solvents, some method abandons the utilization of pueraria starch, these all cause the waste of resource and the pollution of environment, economic benefit is also lower simultaneously.
Summary of the invention
The object of the invention is to provide a kind of method utilizing Pueraria lobota slag to extract puerarin, comprehensive utilization root of kudzu vine resource, and extracting and purifying method is pollution-free, efficiency is higher.
For achieving the above object, adopt technical scheme as follows:
Extract a method for puerarin in Pueraria lobota slag, comprise the following steps:
1) by dry for the Pueraria lobota slag obtained after extraction kudzuvine root starch, micronizing is to particle diameter 1-20 micron;
2) the Pueraria lobota slag after pulverizing mixes with ethanol, and the beta-cyclodextrin added, carries out ultrasonic extraction; Reflux, suction filtration extracts puerarin;
3) by filtrate rotary evaporation to paste, reclaim ethanol, the vacuum-drying of gained medicinal extract simultaneously;
4) supercritical carbon dioxide extraction is carried out to medicinal extract, obtain puerarin.
By such scheme, step 1) Pueraria lobota slag drying temperature is between 40 ~ 60 DEG C.
By such scheme, step 2) pulverize after Pueraria lobota slag and ethanol solid-liquid ratio be 1:(5 ~ 10) g/mL.
By such scheme, step 2) the described ultrasonic extraction time is between 30 ~ 60min, temperature is between 60 ~ 80 DEG C.
By such scheme, step 2) described in Pueraria lobota slag and the mass ratio of beta-cyclodextrin be 1:(0.2 ~ 0.6).
By such scheme, step 2) temperature of described reflux is 80 DEG C.
By such scheme, step 3) temperature of described rotary evaporation is 80 DEG C.
By such scheme, step 3) the vacuum drying temperature of gained medicinal extract is 40 ~ 60 DEG C.
By such scheme, step 4) described supercritical carbon dioxide extraction temperature is 30 ~ 65 DEG C, extracting pressure 8 ~ 17MPa, extraction time 60 ~ 100min.
Beneficial effect of the present invention is:
Pueraria lobota slag is after micronizing, and the dissolution rate of effective constituent puerarin can be significantly improved along with the continuous reduction of powder particle diameter.
Beta-cyclodextrin is with α-1 by 7 glucosyl residues, 4-glycosidic link connects into ring-type, in wide at the top and narrow at the bottom, both ends open, hollow " tubbiness " structure, form the larger inclusion compound of solubleness in the barrel-like structure that puerarin can enter beta-cyclodextrin, thus add the solubleness of puerarin and the speed of stripping from the root of kudzu vine.
Ultrasonic extraction separation and purification puerarin have with short production cycle, efficiency is high, equipment is simple, boiler heat supplying and the advantage such as water coolant is few, energy efficient, reduction environmental pollution, product cost are low.
Supercritical fluid extraction is a kind of new technology just grown up recent years, compares with traditional solvent extraction, and have solute, solvent is easy to be separated, the advantages such as rate of extraction is fast, are specially adapted to extract or exquisite thermo-sensitivity and oxidizable material.Due to extraction agent (CO used 2) be gas, easily remove, products obtained therefrom non-residual toxicity, be specially adapted to medicine and foodstuffs industry.
Embodiment
Following examples explain technical scheme of the present invention further, but not as limiting the scope of the invention.
The process extracting puerarin in Pueraria lobota slag of the present invention is as follows:
1) the Pueraria lobota slag after selection and withdrawal kudzuvine root starch dries rapidly or be placed in loft drier to carry out, and temperature controls below 80 DEG C, and priority acccess control is between 40 ~ 60 DEG C;
2) get a certain amount of dry Pueraria lobota slag powder micronizing, select laboratory special small micronizer mill, particle diameter is 1-20 micron;
3) the Pueraria lobota slag after pulverizing, mix with ethanol, the concentration of ethanol is 70 ~ 75%, and Pueraria lobota slag and amount of alcohol control at 1:(5-10) g/mL;
4) add beta-cyclodextrin fully to stir, the mass ratio of Pueraria lobota slag and beta-cyclodextrin controls at 1:(0.2-0.6);
5) ultrasonic extraction, first carries out single factor experiment, and the factors such as alcohol concn, solid-liquid ratio, ultrasonic extraction time, temperature of investigating, on the impact of puerarin extraction yield, on the basis of single factor experiment, adopt L 9(3 4) carry out orthogonal, with the extraction yield of puerarin for examination index, result shows that optimal processing parameter be alcohol concn is 70%, solid-liquid ratio is 1g:8mL, extraction time 40min, temperature 55 DEG C;
6) after 80 DEG C of water-bath backflow 1h, after suction filtration, filter residue continues backflow repetition 3 times, and filtrate merges;
7) 80 DEG C of rotary evaporations are to paste, and reclaim ethanol, the vacuum-drying of gained medicinal extract, temperature controls below 80 DEG C, and priority acccess control is between 40 ~ 60 DEG C;
8) supercritical CO 2extraction, adopt response phase method to optimize the impact of the conditions such as charging capacity, extracting pressure, extraction temperature extraction time on the puerarin purity extracted, result shows that optimal processing parameter is charging capacity 50g, extraction temperature 55 DEG C, extracting pressure 16MPa, extraction time 90min.
Embodiment 1
1) will extract the Pueraria lobota slag that obtains after kudzuvine root starch 40 DEG C of dryings, micronizing is to particle diameter 1-20 micron;
2) the Pueraria lobota slag after pulverizing mixes with ethanol, and solid-liquid ratio is 1:5g/mL, adds beta-cyclodextrin (mass ratio of Pueraria lobota slag and beta-cyclodextrin is 1:0.2), ultrasonic extraction 30min at temperature 80 DEG C; Reflux at 80 DEG C, suction filtration extracts puerarin;
3) 80 DEG C by filtrate rotary evaporation to paste, reclaim ethanol, gained medicinal extract is 60 DEG C of vacuum-dryings simultaneously;
4) supercritical carbon dioxide extraction is carried out to medicinal extract, extraction temperature is 65 DEG C, namely extracting pressure 8MPa, extraction time 100min obtain puerarin.
With reference to puerarin typical curve, adopt ultraviolet spectrophotometer method, the extraction yield calculating gained puerarin of the present invention is 1.376%, and purity is 81.60%.
Embodiment 2
1) will extract the Pueraria lobota slag that obtains after kudzuvine root starch 60 DEG C of dryings, micronizing is to particle diameter 1-20 micron;
2) the Pueraria lobota slag after pulverizing mixes with ethanol, and solid-liquid ratio is 1:10g/mL, adds beta-cyclodextrin (mass ratio of Pueraria lobota slag and beta-cyclodextrin is 1:0.5), ultrasonic extraction 60min under temperature 60 C; Reflux at 80 DEG C, suction filtration extracts puerarin;
3) 80 DEG C by filtrate rotary evaporation to paste, reclaim ethanol, gained medicinal extract is 40 DEG C of vacuum-dryings simultaneously;
4) supercritical carbon dioxide extraction is carried out to medicinal extract, extraction temperature is 30 DEG C, namely extracting pressure 17MPa, extraction time 60min obtain puerarin.
With reference to puerarin typical curve, adopt ultraviolet spectrophotometer method, the extraction yield calculating gained puerarin of the present invention is 1.483%, and purity is 83.2%.
Embodiment 3
1) will extract the Pueraria lobota slag that obtains after kudzuvine root starch 50 DEG C of dryings, micronizing is to particle diameter 1-20 micron;
2) the Pueraria lobota slag after pulverizing mixes with ethanol, and solid-liquid ratio is 1:8g/mL, adds beta-cyclodextrin (mass ratio of Pueraria lobota slag and beta-cyclodextrin is 1:0.6), ultrasonic extraction 40min at temperature 55 DEG C; Reflux at 80 DEG C, suction filtration extracts puerarin;
3) 80 DEG C by filtrate rotary evaporation to paste, reclaim ethanol, gained medicinal extract is 50 DEG C of vacuum-dryings simultaneously;
4) supercritical carbon dioxide extraction is carried out to medicinal extract, extraction temperature is 60 DEG C, namely extracting pressure 14MPa, extraction time 70min obtain puerarin.
With reference to puerarin typical curve, adopt ultraviolet spectrophotometer method, the extraction yield calculating gained puerarin of the present invention is 1.432%, and purity is 82.2%.

Claims (9)

1. extract a method for puerarin in Pueraria lobota slag, it is characterized in that comprising the following steps:
1) by dry for the Pueraria lobota slag obtained after extraction kudzuvine root starch, micronizing is to particle diameter 1-20 micron;
2) the Pueraria lobota slag after pulverizing mixes with ethanol, and the beta-cyclodextrin added, carries out ultrasonic extraction; Reflux, suction filtration extracts puerarin;
3) by filtrate rotary evaporation to paste, reclaim ethanol, the vacuum-drying of gained medicinal extract simultaneously;
4) supercritical carbon dioxide extraction is carried out to medicinal extract, obtain puerarin.
2. extracting the method for puerarin as claimed in claim 1 in Pueraria lobota slag, it is characterized in that step 1) Pueraria lobota slag drying temperature is between 40 ~ 60 DEG C.
3. extract the method for puerarin as claimed in claim 1 in Pueraria lobota slag, it is characterized in that step 2) pulverize after Pueraria lobota slag and ethanol solid-liquid ratio be 1:(5 ~ 10) g/mL.
4. extract the method for puerarin as claimed in claim 1 in Pueraria lobota slag, it is characterized in that step 2) the described ultrasonic extraction time is between 30 ~ 60min, temperature is between 60 ~ 80 DEG C.
5. extract the method for puerarin as claimed in claim 1 in Pueraria lobota slag, it is characterized in that step 2) described in Pueraria lobota slag and the mass ratio of beta-cyclodextrin be 1:(0.2 ~ 0.6).
6. extract the method for puerarin as claimed in claim 1 in Pueraria lobota slag, it is characterized in that step 2) temperature of described reflux is 80 DEG C.
7. extract the method for puerarin as claimed in claim 1 in Pueraria lobota slag, it is characterized in that step 3) temperature of described rotary evaporation is 80 DEG C.
8. extract the method for puerarin as claimed in claim 1 in Pueraria lobota slag, it is characterized in that step 3) the vacuum drying temperature of gained medicinal extract is 40 ~ 60 DEG C.
9. extract the method for puerarin as claimed in claim 1 in Pueraria lobota slag, it is characterized in that step 4) described supercritical carbon dioxide extraction temperature is 30 ~ 65 DEG C, extracting pressure 8 ~ 17MPa, extraction time 60 ~ 100min.
CN201510183759.2A 2015-04-17 2015-04-17 A kind of method that Puerarin is extracted in Pueraria lobota slag Expired - Fee Related CN104844584B (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105218533A (en) * 2015-10-13 2016-01-06 江西农业大学 A kind of method of simultaneously separation and purification puerarin and daidzein from the root of kudzu vine
CN106036902A (en) * 2016-06-07 2016-10-26 河南科技大学 Preparation method of healthy chenopodium quinoa leaf total flavonoid lozenge
CN108707142A (en) * 2018-06-21 2018-10-26 湖南双晟科技信息咨询有限公司 A kind of Retreatment method of pueraria starch processing slag and effluent
CN108719982A (en) * 2018-05-21 2018-11-02 湖北葛百岁葛业有限公司 Kudzuvine root starch preparation method rich in Puerarin
CN111393422A (en) * 2020-05-07 2020-07-10 四川轻化工大学 Method for producing puerarin from radix Puerariae

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CN103204848A (en) * 2012-01-11 2013-07-17 随州市康汇保健品有限公司 Method for extracting puerarin

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CN1868484A (en) * 2006-06-23 2006-11-29 合肥工业大学 Method and device for high efficiency separation of puerarin
CN103204848A (en) * 2012-01-11 2013-07-17 随州市康汇保健品有限公司 Method for extracting puerarin

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN105218533A (en) * 2015-10-13 2016-01-06 江西农业大学 A kind of method of simultaneously separation and purification puerarin and daidzein from the root of kudzu vine
CN105218533B (en) * 2015-10-13 2018-01-30 江西农业大学 A kind of method for isolating and purifying Puerarin and daidzein simultaneously from the root of kudzu vine
CN106036902A (en) * 2016-06-07 2016-10-26 河南科技大学 Preparation method of healthy chenopodium quinoa leaf total flavonoid lozenge
CN108719982A (en) * 2018-05-21 2018-11-02 湖北葛百岁葛业有限公司 Kudzuvine root starch preparation method rich in Puerarin
CN108707142A (en) * 2018-06-21 2018-10-26 湖南双晟科技信息咨询有限公司 A kind of Retreatment method of pueraria starch processing slag and effluent
CN111393422A (en) * 2020-05-07 2020-07-10 四川轻化工大学 Method for producing puerarin from radix Puerariae

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