CN103254185A - Novel process for producing puerarin by utilizing root of kudzu vine - Google Patents
Novel process for producing puerarin by utilizing root of kudzu vine Download PDFInfo
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- CN103254185A CN103254185A CN2013101978229A CN201310197822A CN103254185A CN 103254185 A CN103254185 A CN 103254185A CN 2013101978229 A CN2013101978229 A CN 2013101978229A CN 201310197822 A CN201310197822 A CN 201310197822A CN 103254185 A CN103254185 A CN 103254185A
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Abstract
The invention provides a novel process for producing puerarin by utilizing root of kudzu vine. According to the process, starch and puerarin in the root of kudzu vine can be respectively extracted. According to the process, the flesh part which is rich in starch and the high-puerarin-content bast part of the root of kudzu vine are separated for performing independent extraction; because puerarin is insoluble in water and soluble in alkaline water, low-alkalinity lime water treatment is adopted in the process of extracting the starch, the content of pueraria root flavone in the starch can be fully kept, and the quality of the edible starch is improved; when puerarin is extracted from the bast part of the root of kudzu vine, non-toxic and safe ethanol serves as a solvent, the extracting process is the traditional reflux extraction process, and coarse puerarin is obtained; and coarse puerarin is subjected to two-step separation, coarse puerarin is subjected to crude separation in the first step through macroporous resin, the purity of puerarin is further improved, puerarin is further refined by employing silica gel column chromatography, and high-purity puerarin with the content of more than or equal to 98 percent is produced. The resources are fully utilized, and the production method is simple and feasible and can be suitable for industrial production.
Description
Technical field
The present invention relates to a kind of novel process of utilizing the root of kudzu vine to produce puerarin, can extract starch and puerarin in the root of kudzu vine respectively.
Background technology
Present most of enterprise all adopts conventional production methods when extracting in the root of kudzu vine puerarin, and concrete operations are as follows.
1. root of kudzu vine pre-treatment: the root of kudzu vine cleans-oven dry-pulverizing.
2. extracting method has three kinds usually, and is specific as follows.
2.1 ultrasonic assisted extraction method: powder of Radix Puerariae → supersound extraction → filtration → concentrating under reduced pressure → mistake post → washing → alcohol is washed → concentrating under reduced pressure → vacuum-drying → puerarin crude extract.
2.2 water extraction method: root of kudzu vine dry powder → water extraction → filtration, filtrate and slag → extract slag → filtration again with the NaOH aqueous solution of concentration 5%, get that silicagel column → washing → 95% ethanol elution → elutriant is evaporated to dried → puerarin on the filtrate → concentrating under reduced pressure → accent pH value → centrifugation → filtrate of twice of filtrate → merging.
2.3 alcohol extracting method: root of kudzu vine dry powder → alcohol reflux → filtration gets the pH value of the filtrate → concentrating under reduced pressure → centrifugation → accent filtrate of twice of filtrate and slag → slag alcohol reflux → filtration again → merging → refilter → filtrate and is concentrated into dried → puerarin.
More than extract the method for puerarin, though can obtain the puerarin crude extract, the operational cycle is long, complex process, and yield is not high yet, and the content of puerarin of gained is not high yet after testing; Most importantly containing a large amount of starch in the root of kudzu vine can not be fully used, and has caused the waste of resource.
Summary of the invention
The present invention proposes the novel process of utilizing the root of kudzu vine to produce puerarin, can extract starch and puerarin in the root of kudzu vine respectively, resource is fully utilized, and improved content, content of puerarin 〉=98%, this technology is simple and easy to do, can be fit to suitability for industrialized production.
The technical solution used in the present invention is as follows: utilize the root of kudzu vine to produce the novel process of puerarin, concrete steps are as follows:
(1). raw materials pretreatment:
Clean the fresh root of kudzu vine, broken apart root of kudzu vine meat portion and phloem then earlier; The phloem oven dry, meat portion is standby; The root of kudzu vine phloem of oven dry is pulverized, got root of kudzu vine bast powder;
(2). the production of pueraria starch:
A. liming soaks: the meat portion in the step (1) is soaked with saturated limewater; Press mass fraction, each part meat portion saturated limewater of 1.5-1.8 part; Soak time is 2-2.5 hour;
B. making beating: the meat portion after soaking and saturated limewater mixture are pulled an oar with hollander, get slurries;
C. adjust pH: being made into mass percent concentration with food grade hydrochloric acid is 5% hydrochloric acid soln, and the pH value of adjusting slurry is to neutral;
D. separate: adopt the method for precipitation, isolate the residue in the slurries, get pueraria starch solution;
E. pass through conventional centrifuge dehydration, oven dry, pulverising step, obtain pueraria starch;
(3). the extraction of puerarin:
1). feed intake: drop into the residue in the root of kudzu vine bast powder in the step (1) and the step (2) in the extractor together;
2). once extract: add 95% ethanol of 5 times of amounts of raw material cumulative volume, 55-60 ℃ of control temperature, refluxing extraction was extracted extracting solution out with pump after 1.5 hours, stayed the dregs of a decoction in the extractor;
3). second extraction: in the dregs of a decoction after once extracting, add 95% ethanol of 4 times of amounts of cumulative volume again, 55-60 ℃ of control temperature, refluxing extraction is extracted extracting solution out with pump after 1.5 hours then;
4). concentrating under reduced pressure: merge twice extracting solution, concentrating under reduced pressure reclaims ethanol, 70 ℃ of control temperature; By the cumulative volume of twice extracting solution, be concentrated into the 25-30% of cumulative volume, get concentrated solution;
5). depositing in water: concentrated solution is added in the crystallizer, add the clear water of 1.5 times of amounts of concentrated solution cumulative volume then, after stirring evenly, placed 1 hour under 55-60 ℃ temperature, filtered while hot is collected filtrate;
6). drying: with filtrate concentrating under reduced pressure again, reclaim ethanol, be concentrated into do not have the alcohol flavor after, remaining liquid is sent into spraying drying, gets the puerarin crude product;
(4). elaboration processing:
1). the pre-treatment of resin: it is after 2.5% sodium hydroxide solution soaks 24 hours that polyamide resin is put into mass percent concentration, cleans to neutral with pure water then; The polyamide resin of handling well is packed in the resin tower;
2). dissolving crude product: fully dissolve the puerarin crude product with 95% ethanol, get puerarin crude product saturated solution;
3). Static Adsorption: puerarin crude product saturated solution is added in the resin tower, left standstill 8-10 hour, carry out ion exchangeable absorption;
4). wash-out: elder generation is washed till colourless with pure water, wash out water and discard; Use 70% ethanol elution then, the ethanol eluate that is washed till outflow is colourless, collects ethanol eluate;
5). concentrate: the concentrating under reduced pressure ethanol eluate, reclaim ethanol, be concentrated into paste;
6). drying: paste adopts vacuum lyophilization, gets the puerarin elaboration;
7). the puerarin elaboration is further purified: adopt silica gel column chromatography, moving phase is used 95% ethanol; With the elutant concentrating under reduced pressure, reclaim ethanol, be concentrated into the 25-30% of elutant cumulative volume, get puerarin elaboration concentrated solution; In puerarin elaboration concentrated solution, the distilled water that adds 4 times of amounts of cumulative volume stirs, and crystallization goes out puerarin, and low-temperature vacuum drying is adopted in centrifuge dehydration then, namely gets content 〉=98% puerarin.
Beneficial effect: the present invention can extract starch and the puerarin in the root of kudzu vine respectively, and resource is fully utilized; Adopt absorption with macroporous adsorbent resin and silica gel column chromatography to make with extra care, obtain content 〉=98% puerarin; This technology is simple and easy to do, can be fit to suitability for industrialized production.
Embodiment
Embodiment 1:
Utilize the root of kudzu vine to produce the novel process of puerarin, concrete steps are as follows:
(1). raw materials pretreatment:
Clean the fresh root of kudzu vine, broken apart root of kudzu vine meat portion and phloem then earlier; The phloem oven dry, meat portion is standby; The root of kudzu vine phloem of oven dry is pulverized, got root of kudzu vine bast powder;
(2). the production of pueraria starch:
A. liming soaks: the meat portion in the step (1) is soaked with saturated limewater; Press mass fraction, each part meat portion is with 1.6 parts saturated limewater; Soak time is 2 hours;
B. making beating: the meat portion after soaking and saturated limewater mixture are pulled an oar with hollander, get slurries; In the pulping process, look the slurries viscosity and add water in right amount and get final product, guarantee the flowability of slurries just, the hollander mesh size is the 6-8 millimeter;
C. adjust pH: being made into mass percent concentration with food grade hydrochloric acid is 5% hydrochloric acid soln, and the pH value of adjusting slurry is to neutral;
D. separate: adopt the method for precipitation, isolate the residue in the slurries, get pueraria starch solution;
E. pass through conventional centrifuge dehydration, oven dry, pulverising step, obtain pueraria starch;
(3). the extraction of puerarin:
1). feed intake: drop into the residue in the root of kudzu vine bast powder in the step (1) and the step (2) in the extractor together;
2). once extract: add 95% ethanol of 5 times of amounts of raw material cumulative volume, 60 ℃ of control temperature, refluxing extraction was extracted extracting solution out with pump after 1.5 hours, stayed the dregs of a decoction in the extractor;
3). second extraction: in the dregs of a decoction after once extracting, add 95% ethanol of 4 times of amounts of cumulative volume again, 60 ℃ of control temperature, refluxing extraction is extracted extracting solution out with pump after 1.5 hours then;
4). concentrating under reduced pressure: merge twice extracting solution, add in the external circulation evaporator and carry out concentrating under reduced pressure, reclaim ethanol, 70 ℃ of control temperature; Cumulative volume by twice extracting solution is concentrated into 30% of cumulative volume, gets concentrated solution;
5). depositing in water: concentrated solution is added in the crystallizer, add the clear water of 1.5 times of amounts of concentrated solution cumulative volume then, after stirring evenly, placed 1 hour under 60 ℃ temperature, filtered while hot is collected filtrate;
6). drying: with filtrate concentrating under reduced pressure again, reclaim ethanol, be concentrated into do not have the alcohol flavor after, remaining liquid is sent into spraying drying, gets the puerarin crude product;
(4). elaboration processing:
1). the pre-treatment of resin: it is after 2.5% sodium hydroxide solution soaks 24 hours that polyamide resin is put into mass percent concentration, cleans to neutral with pure water then; The polyamide resin of handling well is packed in the resin tower;
2). dissolving crude product: fully dissolve the puerarin crude product with 95% ethanol, get puerarin crude product saturated solution;
3). Static Adsorption: puerarin crude product saturated solution is added in the resin tower, left standstill 8 hours, carry out ion exchangeable absorption;
4). wash-out: elder generation is washed till colourless with pure water, wash out water and discard; Use 70% ethanol elution then, the ethanol eluate that is washed till outflow is colourless, collects ethanol eluate;
5). concentrate: the concentrating under reduced pressure ethanol eluate, reclaim ethanol, be concentrated into paste;
6). drying: paste adopts vacuum lyophilization, gets the puerarin elaboration;
7). the puerarin elaboration is further purified: adopt silica gel column chromatography, moving phase is used 95% ethanol; With the elutant concentrating under reduced pressure, reclaim ethanol, be concentrated into 30% of elutant cumulative volume, get puerarin elaboration concentrated solution; In puerarin elaboration concentrated solution, the distilled water that adds 4 times of amounts of cumulative volume stirs, and crystallization goes out puerarin, and low-temperature vacuum drying is adopted in centrifuge dehydration then, namely gets the puerarin of content 〉=98%.
In the above-mentioned Static Adsorption, the consumption of polyamide resin can be determined according to experiment, to one skilled in the art, be easy to determine.The consumption of common polyamide resin: press mass ratio, the puerarin crude product: the ratio of polyamide resin is 1:1-2.5.
Above-mentioned vacuum lyophilization is prior art, and technical parameter is: freezing temp-40 ℃, freezing time 2 hours; 30 ℃ of drying temperatures, vacuum tightness is greater than-0.085MPa, and 3 hours time of drying, finished product is moisture to be not more than 5%.
Silica gel column chromatography also is prior art, uses the chromatographic silica gel (granularity is the 100-200 order) of " Qingdao Haiyang Chemical Manufacture " in the embodiments of the invention 1; At first silica gel 120 ℃ of down activation two hours, put cold back and take out 2/3rds and pack in the glass chromatography column, compress, remaining 1/3rd silica gel mixes the glass chromatography column top of evenly packing into the puerarin elaboration, adds 95% ethanol elution that becomes a mandarin then; Press mass ratio, the puerarin elaboration: the ratio of silica gel is 1:8-10.
Claims (1)
1. utilize the root of kudzu vine to produce the novel process of puerarin, concrete steps are as follows:
(1). raw materials pretreatment:
Clean the fresh root of kudzu vine, broken apart root of kudzu vine meat portion and phloem then earlier; The phloem oven dry, meat portion is standby; The root of kudzu vine phloem of oven dry is pulverized, got root of kudzu vine bast powder;
(2). the production of pueraria starch:
A. liming soaks: the meat portion in the step (1) is soaked with saturated limewater; Press mass fraction, each part meat portion saturated limewater of 1.5-1.8 part; Soak time is 2-2.5 hour;
B. making beating: the meat portion after soaking and saturated limewater mixture are pulled an oar with hollander, get slurries;
C. adjust pH: being made into mass percent concentration with food grade hydrochloric acid is 5% hydrochloric acid soln, and the pH value of adjusting slurry is to neutral;
D. separate: adopt the method for precipitation, isolate the residue in the slurries, get pueraria starch solution;
E. pass through conventional centrifuge dehydration, oven dry, pulverising step, obtain pueraria starch;
(3). the extraction of puerarin:
1). feed intake: drop into the residue in the root of kudzu vine bast powder in the step (1) and the step (2) in the extractor together;
2). once extract: add 95% ethanol of 5 times of amounts of raw material cumulative volume, 55-60 ℃ of control temperature, refluxing extraction was extracted extracting solution out with pump after 1.5 hours, stayed the dregs of a decoction in the extractor;
3). second extraction: in the dregs of a decoction after once extracting, add 95% ethanol of 4 times of amounts of cumulative volume again, 55-60 ℃ of control temperature, refluxing extraction is extracted extracting solution out with pump after 1.5 hours then;
4). concentrating under reduced pressure: merge twice extracting solution, concentrating under reduced pressure reclaims ethanol, 70 ℃ of control temperature; By the cumulative volume of twice extracting solution, be concentrated into the 25-30% of cumulative volume, get concentrated solution;
5). depositing in water: concentrated solution is added in the crystallizer, add the clear water of 1.5 times of amounts of concentrated solution cumulative volume then, after stirring evenly, placed 1 hour under 55-60 ℃ temperature, filtered while hot is collected filtrate;
6). drying: with filtrate concentrating under reduced pressure again, reclaim ethanol, be concentrated into do not have the alcohol flavor after, remaining liquid is sent into spraying drying, gets the puerarin crude product;
(4). elaboration processing:
1). the pre-treatment of resin: it is after 2.5% sodium hydroxide solution soaks 24 hours that polyamide resin is put into mass percent concentration, cleans to neutral with pure water then; The polyamide resin of handling well is packed in the resin tower;
2). dissolving crude product: fully dissolve the puerarin crude product with 95% ethanol, get puerarin crude product saturated solution;
3). Static Adsorption: puerarin crude product saturated solution is added in the resin tower, left standstill 8-10 hour, carry out ion exchangeable absorption;
4). wash-out: elder generation is washed till colourless with pure water, wash out water and discard; Use 70% ethanol elution then, the ethanol eluate that is washed till outflow is colourless, collects ethanol eluate;
5). concentrate: the concentrating under reduced pressure ethanol eluate, reclaim ethanol, be concentrated into paste;
6). drying: paste adopts vacuum lyophilization, gets the puerarin elaboration;
7). the puerarin elaboration is further purified: adopt silica gel column chromatography, moving phase is used 95% ethanol; With the elutant concentrating under reduced pressure, reclaim ethanol, be concentrated into the 25-30% of elutant cumulative volume, get puerarin elaboration concentrated solution; In puerarin elaboration concentrated solution, the distilled water that adds 4 times of amounts of cumulative volume stirs, and crystallization goes out puerarin, and low-temperature vacuum drying is adopted in centrifuge dehydration then, namely gets content 〉=98% puerarin.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864767A (en) * | 2014-03-26 | 2014-06-18 | 南阳理工学院 | Puerarin refining process |
| CN104147101A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Freeze-drying method of lobed kudzuvine roots |
| CN104154711A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Freeze-drying method for preparing high-activity kudzu root decoction pieces |
| CN104873569A (en) * | 2015-06-23 | 2015-09-02 | 四川大学 | Method for efficiently and synchronously extracting pueraria starch and flavone |
| CN107522692A (en) * | 2017-10-25 | 2017-12-29 | 贵州国农葛业有限公司 | A kind of method that waste liquid separating puerarin is produced using pueraria starch |
| CN113683589A (en) * | 2021-09-06 | 2021-11-23 | 福州鼓楼区云珀生物科技有限公司 | Extraction method and application of pueraria isoflavone |
| CN115530352A (en) * | 2022-09-13 | 2022-12-30 | 淄博杜隆商贸有限公司 | Seasoning salt containing radix Puerariae extract and having uric acid lowering effect, and its preparation method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103864767A (en) * | 2014-03-26 | 2014-06-18 | 南阳理工学院 | Puerarin refining process |
| CN104147101A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Freeze-drying method of lobed kudzuvine roots |
| CN104154711A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Freeze-drying method for preparing high-activity kudzu root decoction pieces |
| CN104873569A (en) * | 2015-06-23 | 2015-09-02 | 四川大学 | Method for efficiently and synchronously extracting pueraria starch and flavone |
| CN107522692A (en) * | 2017-10-25 | 2017-12-29 | 贵州国农葛业有限公司 | A kind of method that waste liquid separating puerarin is produced using pueraria starch |
| CN113683589A (en) * | 2021-09-06 | 2021-11-23 | 福州鼓楼区云珀生物科技有限公司 | Extraction method and application of pueraria isoflavone |
| CN115530352A (en) * | 2022-09-13 | 2022-12-30 | 淄博杜隆商贸有限公司 | Seasoning salt containing radix Puerariae extract and having uric acid lowering effect, and its preparation method |
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Application publication date: 20130821 |