CN102961436A - Method for rapidly extracting pueraria isoflavones from pueraria waste - Google Patents
Method for rapidly extracting pueraria isoflavones from pueraria waste Download PDFInfo
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- CN102961436A CN102961436A CN2012105305079A CN201210530507A CN102961436A CN 102961436 A CN102961436 A CN 102961436A CN 2012105305079 A CN2012105305079 A CN 2012105305079A CN 201210530507 A CN201210530507 A CN 201210530507A CN 102961436 A CN102961436 A CN 102961436A
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- radix puerariae
- pueraria
- isoflavone
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Abstract
The invention relates to a method for rapidly extracting pueraria isoflavones from pueraria waste. The method specifically comprises the following steps of: (1) crushing the pueraria waste, puffing by adopting liquid state CO2; (2) secondarily extracting the puffed pueraria waste by adopting supersonic waves, mixing extracting solutions of two times, and obtaining clear liquid through filtering and centrifuging; and (3) carrying out vacuum concentration on the clear liquid, and freeze-drying to obtain a crude product of pueraria isoflavones, wherein the purity of the pueraria isoflavones is not less than 11percent, and the extraction ratio of isoflavone is not less than 92 percent. The method has advantages of short extracting time, little solvent consumption, and low extracting cost.
Description
Technical field
The present invention relates to a kind of from the Radix Puerariae dead meal method of high efficiency extraction Radix Puerariae isoflavone, be a kind of liquid CO that uses
2Expanded Radix Puerariae dead meal obtains the new method of Radix Puerariae isoflavone again by ultrasonic extraction.
Background technology
Radix Puerariae isoflavone (being mainly puerarin) is the main active of Radix Puerariae; Have arrhythmia, blood fat reducing, expansion of cerebral vascular, increase cerebral blood flow, improve the multiple pharmacological effect such as microcirculation, its good effect and be widely used in clinically the treatments such as cardiovascular and cerebrovascular disease, hyperlipidemia, diabetes.In the powder of Radix Puerariae production process in the most of areas of China, the slag charge that Radix Puerariae is washed behind the powder goes out of use, and thinks and has no value.But contain a large amount of Radix Puerariae isoflavones in these waste residues (fibrous matter) exactly, it is enriched in the fiber.The analysis showed that, more than 60% of Radix Puerariae isoflavone station total amount in the waste residue, content is about about 25% in the powder of Radix Puerariae, also has on a small quantity to run off in processing powder of Radix Puerariae process.So utilizing the Radix Puerariae dead meal to extract Radix Puerariae isoflavone is important source of puerarin.Domestic relevant for extraction Radix Puerariae isoflavone bibliographical information: Zhao Haoru etc. extract Radix Puerariae total flavoness with four kinds of methods such as percolations; Li Furongs etc. use microwave technology to extract total flavones first from Radix Puerariae; The single factor of the employings such as Liu Huoan and orthogonal test are optimized the process conditions of extracting Radix Puerariae total flavones, show that optimum process condition is with 30% ethanol extraction of 9 times of amounts 3 times, each 1h; More than these methods all be directly to extract with Radix Puerariae (containing a large amount of Radix Puerariae starch), but not wash the Radix Puerariae dead meal behind the powder, not only wasted powder of Radix Puerariae, in leaching process, also strengthened consumption and the extraction time of extracting solvent.Utilize the Radix Puerariae waste residue to extract the domestic also bibliographical information of Radix Puerariae isoflavone: Shi Yingying etc. combine the enzyme process pretreatment of Radix Puerariae slag with the ethanol extraction process, with the Radix Puerariae slag 10g of diameter 3mm, in the 250mL triangular flask.Cellulase or xylanase treatment by doses.Solid-liquid ratio is 1: 15, pH value 4.8,50 ℃ are lower process a period of time after, the extraction ratio that filters, measures the isoflavone content isoflavone in the enzymolysis solution is significantly improved; When the cellulase consumption is 10FPIU, process 12h after, the total isoflavone yield can increase to 1.14%, is 1.36 times of conventional alcohol extracting method; Be under the condition of 300IU at the xylanase consumption, process 6h after, total isoflavone yield 1.28% is 1.52 times of conventional alcohol extracting method; The residue after with the Radix Puerariae separating starch such as Zuo Leilei is used for extracting Radix Puerariae isoflavone, has realized the comprehensive utilization of raw material and the saving of solvent and the energy; And obtained the optimum condition of isoflavone in the ultrasonic assisted extraction Radix Puerariae residue by the research of single factor, orthogonal experiment: extraction temperature is 60 ℃, solvent is 60%(V/V) alcoholic solution, solid-liquid ratio is 1:18, extraction time is 30min, ultrasonic power 250W, supersonic frequency 40KHz; Once extract under this condition, the isoflavone extraction ratio is 88.3%, and the crude extract yield is 8.4%, and its isoflavone purity is 10.7%.There is certain defect in these extracting method, namely because Radix Puerariae isoflavone is contained in these fibers and is difficult to stripping, need to consume a large amount of solvents, and extraction time long (or enzyme processing time is long), the relative cost in lower, the production process of extraction ratio is high simultaneously.
Summary of the invention
In order to solve the existing problem that solvent-oil ratio is large, extraction time is long, extraction ratio is relatively low that Radix Puerariae isoflavone exists of from the Radix Puerariae dead meal, extracting, the invention provides a kind of yield high, use the few method of rapid extraction Radix Puerariae isoflavone from the Radix Puerariae dead meal of solvent.
Concrete preparation method of the present invention is as follows:
The concrete operation step of rapid extraction Radix Puerariae isoflavone is as follows from the Radix Puerariae dead meal:
(1). the Radix Puerariae dead meal of drying is pulverized, and crossed 20 mesh sieves, in the pressurized tank of packing into, open air intake valve and inject liquid CO
2, make the tank internal pressure reach 7MPa and kept 30 minutes, open the valve of giving vent to anger and unload rapidly and be pressed onto normal pressure, take out puffing material;
(2). puffing material is added extraction pot, and add the ethanol of concentration 60%, be warmed up to 50 ℃, stir and be aided with ultrasonic extraction 15min, melt cinder separates; In slag charge, add again the ethanol of concentration 60%, carry out extracting the second time 10min; The extracting solution that merges secondary, after filtration, tubular type is centrifugal, obtains clear liquid;
(3). clear liquid is carried out concentrating under reduced pressure, concentrated vacuum is-0.08MPa～-0.1 MPa, temperature is 65 ℃, be concentrated into 1/8～1/10 of original volume, obtain concentrated solution, again concentrated solution is carried out lyophilization, obtain the crude product Radix Puerariae isoflavone, the purity of Radix Puerariae isoflavone 〉=11% wherein, isoflavone extraction ratio 〉=92%.
The present invention adopts liquid CO
2Expanded Radix Puerariae dead meal extracts Radix Puerariae isoflavone with the method for ultrasound wave secondary rapid extraction again, extraction time short (25 minutes), and solvent load few (solid-liquid ratio is 1:8), products obtained therefrom purity is 〉=11%: isoflavone extraction ratio 〉=92%.The Radix Puerariae resource is fully used.
The present invention adopts liquid CO in operating process
2Moment expanded Radix Puerariae dead meal, almost completely " exposure " out to make the Radix Puerariae isoflavone that is enriched in the fibrous tissue, Fast Stripping is in alcoholic solution under ultrasound wave is auxiliary, the speed and the extraction ratio that extract have been improved, and owing to there is not high temperature (extruding puffing needs high temperature usually), the character of Radix Puerariae isoflavone without destroying infection, has been guaranteed product quality preferably.
The specific embodiment
Below in conjunction with embodiment, the present invention is further described.
Embodiment 1
The concrete operation step of rapid extraction Radix Puerariae isoflavone is as follows from the Radix Puerariae dead meal:
(1) gets 200 grams through pulverizing and cross the Radix Puerariae dead meal of 20 mesh sieves, (can use supercritical CO in the 1L pressurized tank of packing into
2Extractor), open air intake valve and inject liquid CO
2, make the tank internal pressure reach 7MPa and kept 30 minutes, open the valve of giving vent to anger and unload rapidly and be pressed onto normal pressure, take out puffing material;
(2) puffing material is added extraction pot, and adds 900 milliliters 60% ethanol, be warmed up to 50 ℃ after, stir and be aided with ultrasonic extraction, extraction time is to carry out melt cinder after 15 minutes to separate.60% the ethanol that adds again 700 milliliters in slag charge carries out extracting 10min the second time; Merge extractive liquid,, after filtration, tubular type after centrifugal clear liquid;
(3) clear liquid is carried out concentrating under reduced pressure, concentrated vacuum is-0.08MPa that temperature is 65 ℃, obtain 120 milliliters of concentrated solutions, concentrated solution is carried out lyophilization again and obtain 16.9 gram crude product Radix Puerariae isoflavones, the purity of its Radix Puerariae isoflavone is 12.1%, isoflavone extraction rate reached to 92.6%.
Embodiment 2
The concrete operation step of rapid extraction Radix Puerariae isoflavone is as follows from the Radix Puerariae dead meal:
(1) gets 200 grams through pulverizing and cross the Radix Puerariae dead meal of 20 mesh sieves, (can use the SCF-CO 2 tank) in the 1L pressurized tank of packing into, open air intake valve and inject liquid CO
2, make the tank internal pressure reach 7.5MPa and kept 15 minutes, open the valve of giving vent to anger and unload rapidly and be pressed onto normal pressure, take out puffing material;
(2) puffing material is added extraction pot, and adds 900 milliliters 60% ethanol, be warmed up to 55 ℃ after, stir and be aided with ultrasonic extraction, extraction time is to carry out melt cinder after 20 minutes to separate.The ethanol that adds again 700 milliliter 60% in slag charge carries out extracting 10min the second time; Merge extractive liquid,, after filtration, tubular type after centrifugal clear liquid;
(3) clear liquid is carried out concentrating under reduced pressure, concentrated vacuum is-0.1MPa that temperature is 65 ℃, obtain 120 milliliters of concentrated solutions, concentrated solution is carried out lyophilization again and obtain 17.6 gram crude product Radix Puerariae isoflavones, the purity of its Radix Puerariae isoflavone is 11.6%, isoflavone extraction rate reached to 93.05%.
Embodiment 3
The concrete operation step of rapid extraction Radix Puerariae isoflavone is as follows from the Radix Puerariae dead meal:
(1) gets 200 grams through pulverizing and cross the Radix Puerariae dead meal of 20 mesh sieves, (can use supercritical CO in the 1L pressurized tank of packing into
2Extractor), open air intake valve and inject liquid CO
2, make the tank internal pressure reach 7.5MPa and kept 15 minutes, open the valve of giving vent to anger and unload rapidly and be pressed onto normal pressure, take out puffing material;
(2) puffing material is added extraction pot, and adds 900 milliliters 60% ethanol, be warmed up to 53 ℃ after, stir and be aided with ultrasonic extraction, extraction time is to carry out melt cinder after 18 minutes to separate.The ethanol that adds again 700 milliliter 60% in slag charge carries out extracting 10min the second time; Merge extractive liquid,, after filtration, tubular type after centrifugal clear liquid;
(3) clear liquid is carried out concentrating under reduced pressure, concentrated vacuum is-0.09 MPa, and temperature is 65 ℃, obtain 120 milliliters of concentrated solutions, concentrated solution is carried out lyophilization again and obtain 17.2 gram crude product Radix Puerariae isoflavones, the purity of its Radix Puerariae isoflavone is 11.8%, isoflavone extraction rate reached to 92.5%.
Claims (1)
1. the method for rapid extraction Radix Puerariae isoflavone from the Radix Puerariae dead meal is characterized in that concrete operation step is as follows:
(1) the Radix Puerariae dead meal of drying is pulverized, and crossed 20 mesh sieves, in the pressurized tank of packing into, open air intake valve and inject liquid CO
2, make the tank internal pressure reach 7MPa and kept 30 minutes, open the valve of giving vent to anger and unload rapidly and be pressed onto normal pressure, take out puffing material;
(2) puffing material is added extraction pot, and add the ethanol of concentration 60%, be warmed up to 50 ℃, stir and be aided with ultrasonic extraction 15min, melt cinder separates; In slag charge, add again the ethanol of concentration 60%, carry out extracting the second time 10min; The extracting solution that merges secondary, after filtration, tubular type is centrifugal, obtains clear liquid;
(3) clear liquid is carried out concentrating under reduced pressure, concentrated vacuum is-0.08MPa～-0.1 MPa, temperature is 65 ℃, be concentrated into 1/8～1/10 of original volume, obtain concentrated solution, again concentrated solution is carried out lyophilization, obtain the crude product Radix Puerariae isoflavone, the purity of Radix Puerariae isoflavone 〉=11% wherein, isoflavone extraction ratio 〉=92%.
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| CN2012105305079A CN102961436A (en) | 2012-12-11 | 2012-12-11 | Method for rapidly extracting pueraria isoflavones from pueraria waste |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110870565A (en) * | 2018-09-04 | 2020-03-10 | 天津星宇航天生物科技有限公司 | A nutraceutical product suitable for astronauts for resisting aging |
| CN111990657A (en) * | 2020-07-14 | 2020-11-27 | 浙江师范大学行知学院 | Process for preparing functional food by utilizing natural selenium-rich radix puerariae residues |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483459A (en) * | 2003-06-23 | 2004-03-24 | 魏长霖 | Puffing preparation method for raw material of Chinese herbl medicine |
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- 2012-12-11 CN CN2012105305079A patent/CN102961436A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1483459A (en) * | 2003-06-23 | 2004-03-24 | 魏长霖 | Puffing preparation method for raw material of Chinese herbl medicine |
Non-Patent Citations (1)
| Title |
|---|
| 左蕾蕾，等: "葛根综合利用与超声辅助提取葛根异黄酮工艺的研究", 《食品与发酵科技》, vol. 47, no. 4, 31 August 2011 (2011-08-31), pages 60 - 63 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110870565A (en) * | 2018-09-04 | 2020-03-10 | 天津星宇航天生物科技有限公司 | A nutraceutical product suitable for astronauts for resisting aging |
| CN111990657A (en) * | 2020-07-14 | 2020-11-27 | 浙江师范大学行知学院 | Process for preparing functional food by utilizing natural selenium-rich radix puerariae residues |
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Application publication date: 20130313 |