CN103772523A - New technology for preparing poria polysaccharide extract through membrane separation and purification technology - Google Patents
New technology for preparing poria polysaccharide extract through membrane separation and purification technology Download PDFInfo
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- CN103772523A CN103772523A CN201410015582.0A CN201410015582A CN103772523A CN 103772523 A CN103772523 A CN 103772523A CN 201410015582 A CN201410015582 A CN 201410015582A CN 103772523 A CN103772523 A CN 103772523A
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Abstract
The invention relates to a new technology for preparing poria polysaccharide extract through membrane separation and purification technology. The technology comprises the following steps: (1) grinding and sieving poria powder into crude powder with 20 meshes, and then adding five to ten times of deionized water to obtain feed liquor; (2) filtering the feed liquor obtained in the step (1) through a centrifugal machine; (3) filtering the filtrate obtained in the step (2) through a micro-filtering membrane PP cotton; (4) further filtering the filtrate through the polysulfone hollow fiber type ultrafiltration film with nominal molecular weight cutoff of 10000 dalton; (5) drying the filtrate obtained in the step (4) in a vacuum freeze-drying manner; (6) carrying out anti-oxidization and anti-aging research to the poria polysaccharide by taking a drosophila as an animal model; (7) carrying out hypoglycemic action research by adopting an in-vitro alpha-glucosidase inhibition model through the poria polysaccharide prepared in the step (5). The new technology is simple to operate, and capable of greatly increasing the purity and efficiency of polysaccharide.
Description
Technical field
The invention belongs to natural product extraction and separation technology field.Invention relates to a kind of extraction separation and purification method of preparing Pachymose take Poria cocos as raw material, and hypoglycemic and effect evaluation anti-oxidant activity.
Background technology
Poria cocos belongs to Aphyllophorales polyporaceae Poria cocos and belongs to, and is Mycophyta Chinese medicine.Taste is sweet, light, flat, the thoughts of returning home, spleen, kidney channel, has the effect such as promoting diuresis to eliminate damp pathogen, invigorating the spleen Ning Xin.Main pharmacodynamics composition in Poria cocos is Pachymose.Pachymose has antitumor, antiviral, anti-oxidant, enhancing body immunizing power, protect the liver, the effect such as hypnosis, anti-inflammatory, niter, can be widely used in the field such as health care, food.Thereby Pachymose can be used for the research and development of antitumor drug for the treatment of tumour, cancer provides new method, also can be used as immunostimulant, for exploitation and the development of healthcare products.The production technique of Pachymose has a lot, current water extraction and alcohol precipitation method, the alkali of mostly adopting is both at home and abroad proposed alcohol deposition method, microwave ultrasonic wave auxiliary law, the extraction of fermentation alcohol deposition method, further by methods such as quaternary salt deposit method, the distribution precipitator method, gel chromatographies, Pachymose is carried out to separation and purification again, become one-component polysaccharide.Current extraction and separation method, although have the advantages such as inexpensive, nontoxic, operational safety, extraction time is long and extraction yield is lower, can not obtain the Pachymose of effective single component.
Extraction and separation method of the present invention is to adopt ultrasonic auxiliary adverse current to boil extracting method to replace traditional leach extraction method, and separates and prepare Pachymose in conjunction with Integrated Films.Extraction of the present invention, membrane sepn impurity elimination purifying process have simple process, extraction yield is high, and good product quality, the significant advantage of comprehensive benefit are applicable to factory's extension and produce.
Summary of the invention
The main technical problem to be solved in the present invention is:
(1) provide a kind of effectively deionized water lixiviate novel method high efficiency extraction Pachymose;
(2) provide a kind of new membrane isolation technique separation and purification Pachymose, this technique has simple to operate, mild condition, and separation efficiency is high, has become the important means of separation of polysaccharides purifying research.
The present invention is achieved through the following technical solutions:
The ancillary technique of a kind of effective deionized water lixiviate novel method utilization is ultrasonic or microwave;
The lixiviate novel process of a kind of effective deionized water lixiviate novel method utilization is boiled and is carried for adverse current;
A kind of film separating system for Pachymose separation and purification divides by molecular weight cut-off or aperture:
Microfiltration ceramic membrane 0.1 μ m
Microfiltration membrane PP cotton 1～10 μ m
Ultra-filtration membrane 10000～30000
A technique for membrane separation purification Pachymose, described technique comprises the following steps:
(1) Poria cocos is crushed and screened into 20 order meal, then adds the deionized water of 5～10 times, ultrasonic adverse current heated and boiled 100min; Ultrasonic power 0.5～20 MHz, leaching process discontinuous stirs raw material, and controlling cooling rate is 1～10 ℃/h, then leaves and takes feed liquid; Continue to boil according to the same terms and carry three times, merge four times feed liquid;
(2) feed liquid step (1) being obtained is filtered through whizzer, removes the impurity below 200 orders, and feed liquid is cooled to below 30 ℃;
(3) filtrate step (2) being obtained is filtered with microfiltration membrane PP is cotton, 25～35 ℃ of service temperatures, pressure 0.1～0.5Mpa;
(4) filtrate step (3) being obtained is that 10000 daltonian polysulfone hollow fibre formula ultra-filtration membranes (UF) further filter with nominal molecular weight cut-off, 25～35 ℃ of service temperatures, pressure 0.05～0.1Mpa;
(5) step (4) gained filtrate is dried by the mode of vacuum lyophilization;
(6) Pachymose of being prepared by step (5), take fruit bat as animal model, carries out anti-oxidant anti-aging research.
(7) Pachymose of being prepared by step (5), adopts external alpha-glucosidase inhibition to carry out enzyme inhibition activity research.
Described technique also comprises from step (1) all carries out to step (5) in encloses container.
Described technique also comprises:
(1): the micro-filtration in step (3) comprises that aperture is cellulose membrane, ceramic membrane or the PP cotton of 0.1～10 μ m.
(2): the ultra-filtration membrane in step (4) is that nominal molecular weight cut-off is 10000 dalton's polysulfones or polypropylene ultra-filtration membrane.
Described production technique adopts lyophilize or spraying concentrated solution dry or that cryogenic vacuum belt drying obtains step (4) to be dried.
beneficial effect of the present invention:ultrasonic auxiliary adverse current used in the present invention is boiled extracting method can significantly shorten extraction time, increases the extraction yield of effective constituent, reduces the stripping of impurity.The method is not subject to the restriction of effective compositional polarity, molecular size range, accelerates the efficient stripping fully of soluble material effective constituent, diffusion.The membrane separating and purifying process that the present invention adopts can have the materials such as high molecular weight protein in effective removal Pachymose, polyphenol, pigment, and compare with decoloring method with traditional albumen that removes, simple to operate, mild condition, not only can avoid Pachymose activity decreased in operating process, also greatly improve the purity of polysaccharide, also improved the efficiency of the further separation and purification of polysaccharide.
Embodiment
embodiment 1
Get Poria cocos 5kg, drop into pot for solvent extraction, add after deionized water 30kg, seal, controlling temperature is 90 ℃, assisting ultrasonic wave power is 10 MHz, and intermittent stirring per hour 5 minutes, after lixiviate 80min, leach filtrate, add respectively again 10kg deionized water to carry out three times times and extract (boil at every turn and carry 30min), merge four leach cooking liquids and after whizzer coarse filtration, leach altogether 55kg, be cooled to 30 ℃; Be cotton filtration of microfiltration membrane PP of 5 μ m with aperture by filtrate, 25 ℃ of service temperatures, pressure 0.3Mpa, obtains filtrate 51kg; The filtrate obtaining is further filtered with the daltonian polysulphones hyperfiltration membrane PS-10 of nominal molecular weight cut-off 10000,25 ℃ of service temperatures, and pressure 0.05Mpa, obtains filtrate 49kg; After filtrate is concentrated, obtain Pachymose powder 3.7kg through lyophilize.
embodiment 2
Get Poria cocos 10kg, extraction agent 100kg, and drop into extractor, controlling temperature is 95 ℃, assisting ultrasonic wave power is 15 MHz, intermittent stirring per hour 10 minutes, and lixiviate, after 100min, leach filtrate, then add 50kg extraction agent to extract 100min, after extracted twice liquid merges, impurity is removed in centrifuging; Filtrate 146kg is cooled to after 30 ℃, is cotton filtration of microfiltration membrane PP of 10 μ m with aperture, 30 ℃ of service temperatures, and pressure 0.5Mpa, obtains filtrate 143kg; Filtrate is further filtered with the daltonian rolling polypropylene of nominal molecular weight cut-off 30000 ultra-filtration membrane HPS-30,30 ℃ of service temperatures, pressure 0.2Mpa, obtains filtrate 138kg; After filtrate is concentrated, obtain crocin powder 7.8kg through lyophilize.
Claims (7)
1. membrane separation and purification technology is prepared a Pachymose extract novel process, and it comprises, and deionization poach is carried, centrifuging, Integrated Films separate; It is characterized in that: comprise the following steps:
(1) deionization poach is carried: Poria cocos is crushed and screened into 20 order meal, then adds the deionized water of 5～10 times, ultrasonic adverse current heated and boiled 100min, extracts 4 times;
(2) centrifugal removal of impurities: extracting solution is carried out to separation, impurity removal, merging filtrate through whizzer;
(3) microfiltration membrane is removed macromole impurity: the filtrate after whizzer separation, impurity removal, filter 25～35 ℃ of service temperatures, pressure 0.1～0.5Mpa with microfiltration membrane PP is cotton;
(4) ultra-filtration membrane separates Pachymose: the filtrate that (3) are obtained is that 10000 daltonian polysulfone hollow fibre formula ultra-filtration membranes (UF) further filter with nominal molecular weight cut-off, 25～35 ℃ of service temperatures, pressure 0.05～0.1Mpa;
(5) product is dry: step (4) gained filtrate is dried by the mode of vacuum lyophilization;
(6) Pachymose antioxygenation: Pachymose prepared by step (5), take fruit bat as animal model, carries out anti-oxidant anti-aging research;
(7) Pachymose hypoglycemic activity: Pachymose prepared by step (5), adopts external alpha-glucosidase inhibition to carry out hypoglycemic activity research.
2. a kind of membrane separation and purification technology according to claim 1 is prepared Pachymose extract novel process, it is characterized in that in step (1), ultrasonic adverse current is boiled extracting method, and its special type is that described method is ultrasonic auxiliary deionized water countercurrent extraction of boiling.
3. a kind of membrane separation and purification technology according to claim 1 is prepared Pachymose extract novel process, it is characterized in that whizzer in step (2), and the whizzer described in it is characterized in that is selected from dull and stereotyped whizzer, horizontal centrifuge and disk centrifugal separator.
4. a kind of membrane separation and purification technology according to claim 1 is prepared Pachymose extract novel process, it is characterized in that the film system in step (3), it is characterized in that film used is microfiltration ceramic membrane, micro-filtration PP cotton, hollow type fiber ultrafiltration membrane or rolling ultrafiltration membrane.
5. a kind of membrane separation and purification technology according to claim 1 is prepared Pachymose extract novel process, it is characterized in that the drying mode in step (5) is that lyophilize or spraying are dry.
6. a kind of membrane separation and purification technology according to claim 1 is prepared Pachymose extract novel process, it is characterized in that the Study on antioxidation in step (6), take fruit bat as animal model, carries out anti-oxidant anti-aging research by the Pachymose of feeding.
7. a kind of membrane separation and purification technology according to claim 1 is prepared Pachymose extract novel process, it is characterized in that the hypoglycemic activity research in step (7), it is characterized in that adopting external alpha-glucosidase inhibition to carry out hypoglycemic activity research.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892784A (en) * | 2015-05-18 | 2015-09-09 | 上海应用技术学院 | A purification method of potentilla anserina polysaccharides |
| CN105061627A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Pachymaran extraction method |
| CN106046192A (en) * | 2016-07-20 | 2016-10-26 | 潜山县三新茶叶专业合作社 | Process for extracting pachyman from poria coccus wolf |
| CN107801981A (en) * | 2017-10-19 | 2018-03-16 | 广州泽力医药科技有限公司 | Gel-type Poria cocos product and its preparation method and application |
| CN108976312A (en) * | 2018-08-27 | 2018-12-11 | 杨鑫 | A kind of method for extraction and purification of pachymaran and application |
| CN109567192A (en) * | 2018-11-16 | 2019-04-05 | 湖南朗林生物资源股份有限公司 | A kind of preparation method of Eurycoma longifolia extract product |
| CN109998009A (en) * | 2018-10-11 | 2019-07-12 | 浙江杏林堂生物科技有限公司 | A kind of solid beverage of Chinese chestnut peptide and preparation method thereof |
| CN110467683A (en) * | 2018-05-09 | 2019-11-19 | 常州柚盾实业投资有限公司 | The preparation method of the alcohol hypostasis of plant or fungi |
| CN111349181A (en) * | 2020-04-03 | 2020-06-30 | 广东一方制药有限公司 | Pachymaran extraction method, pachymaran extract and poria product combined production process |
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| CN103214533A (en) * | 2013-04-19 | 2013-07-24 | 湖南农业大学 | Method for continuously preparing cordycepin and cordyceps polysaccharide by using membrane separation technology |
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| CN103288975A (en) * | 2013-05-13 | 2013-09-11 | 茅兴娟 | Extracting method for refining astragalus polysaccharide |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104892784A (en) * | 2015-05-18 | 2015-09-09 | 上海应用技术学院 | A purification method of potentilla anserina polysaccharides |
| CN104892784B (en) * | 2015-05-18 | 2017-05-31 | 上海应用技术学院 | A kind of method of purification of fern amylose |
| CN105061627A (en) * | 2015-08-31 | 2015-11-18 | 桂林茗兴生物科技有限公司 | Pachymaran extraction method |
| CN106046192A (en) * | 2016-07-20 | 2016-10-26 | 潜山县三新茶叶专业合作社 | Process for extracting pachyman from poria coccus wolf |
| CN107801981A (en) * | 2017-10-19 | 2018-03-16 | 广州泽力医药科技有限公司 | Gel-type Poria cocos product and its preparation method and application |
| CN107801981B (en) * | 2017-10-19 | 2020-09-29 | 广州泽力医药科技有限公司 | Gel type poria cocos product and preparation method and application thereof |
| CN110467683A (en) * | 2018-05-09 | 2019-11-19 | 常州柚盾实业投资有限公司 | The preparation method of the alcohol hypostasis of plant or fungi |
| CN108976312A (en) * | 2018-08-27 | 2018-12-11 | 杨鑫 | A kind of method for extraction and purification of pachymaran and application |
| CN109998009A (en) * | 2018-10-11 | 2019-07-12 | 浙江杏林堂生物科技有限公司 | A kind of solid beverage of Chinese chestnut peptide and preparation method thereof |
| CN109567192A (en) * | 2018-11-16 | 2019-04-05 | 湖南朗林生物资源股份有限公司 | A kind of preparation method of Eurycoma longifolia extract product |
| CN111349181A (en) * | 2020-04-03 | 2020-06-30 | 广东一方制药有限公司 | Pachymaran extraction method, pachymaran extract and poria product combined production process |
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| CN103772523B (en) | 2016-02-10 |
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Effective date of registration: 20161216 Address after: 430000 Hubei Development Zone, East Lake high tech Avenue, No. 666 Wuhan national biological industry base project B, C, D District R & D building Patentee after: WUHAN HUANG MEDICAL SYSTEM BIOLOGICAL MEDICINE INC. Address before: 430075 858 (A-7# ) Patentee before: WUHAN NEW GUOFENG TECHNOLOGY DEVELOPMENT CO., LTD. |