CN103554284A - Extraction and separation process for peony stamen polysaccharide - Google Patents
Extraction and separation process for peony stamen polysaccharide Download PDFInfo
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- CN103554284A CN103554284A CN201310471886.3A CN201310471886A CN103554284A CN 103554284 A CN103554284 A CN 103554284A CN 201310471886 A CN201310471886 A CN 201310471886A CN 103554284 A CN103554284 A CN 103554284A
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Abstract
The invention discloses an extraction and separation process for peony stamen polysaccharide. The extraction and separation process comprises the following steps of (1) smashing; (2) breaking cell walls; (3) degreasing and removing oligosaccharide; (4) extracting polysaccharide; (5) removing protein by a sevage method; (6) dialyzing to remove salt and other small molecule compounds, concentrating dialysate under a reduced pressure to obtain a concentrated solution; (7) precipitating polysaccharide and drying, vacuum freeze-drying the collected precipitate, and thus the peony stamen polysaccharide is obtained. The extraction and separation process is simple, practical and controllable. The yield of peony stamen polysaccharide can reach 3.1% and an extraction rate can reach 62.6%.
Description
Technical field
The present invention relates to a kind of extraction of biologically active substance with separated, specifically refer to the extraction and separation process of tree peony stamen polysaccharide.
Background technology
Tree peony originates in the western part of China Qinling Mountains and Daba Mountain one band, except as ornamental plant, also can be used for producing the root bark of tree peony and is used as medicine, and has the drug effects such as the cardiovascular disorder of improvement, calmness, anti-inflammatory and raising immunity of organisms.
Polysaccharide is at occurring in nature rich content, has significant immunoregulation effect, antitumor, hypoglycemic and antivirus action etc., caused the great attention of domestic and international medical circle, becomes the focus of Recent study and application.Among the peoplely because having effects such as reducing blood fat, prevention and adjuvant therapy of heart cerebrovascular diseases, tree peony stamen tea enjoy people to pay close attention to, because of it, gastrointestinal dysfunction, constipation are had to positive auxiliary therapeutic action simultaneously, prostatitis, prostatomegaly are had to assisting therapy and restitution, be described as " plant gold ".The extraction separation of tree peony stamen and pharmacological research are had no to document and patent report both at home and abroad.Therefore, from tree peony stamen, extract separating polyose, can promote using value and the economic worth of tree peony, significant to the comprehensive utilization of tree peony.
Summary of the invention
One of the technical problem to be solved in the present invention is to extract separating polyose from tree peony stamen.Another technical problem that the present invention will solve is the system extraction and separation process method adopting in order to obtain tree peony stamen polysaccharide.For solving the problems of the technologies described above, the present invention has studied and defined following technical scheme.
1) pulverize: gather tree peony stamen, after 40～50 ℃ of oven dry, pulverize, cross 20～100 mesh sieves.
2) cell wall breaking: the water to adding 5～15 times of amounts in the tree peony stamen of pulverizing, stir, be placed in Ultralow Temperature Freezer (20～-40 ℃) freezing 12～16 hours.Drop in 70～90 ℃ of water-baths and thaw, water-bath 1～2 hour.Then 200W supersound process is 10～50 minutes, filters to such an extent that solid substance is broken wall stamen.
3) degreasing, except oligosaccharides: the tree peony stamen after broken wall adds sherwood oil to reflux 6～8 hours, and solid-liquid ratio is 1 ︰ 2～4 (W/V), and solid substance (degreasing tree peony stamen) is filtered to obtain in lixiviate degreasing.In solid substance, add 80% ethanol, solid-liquid ratio is 1 ︰ 2～4 (W/V), refluxes 6～8 hours, and suction filtration, to remove oligosaccharides.Repeat 1～3 time, suction filtration obtains solid substance (degreasing, except the tree peony stamen after oligosaccharides).
4) extraction of polysaccharide: add distilled water in solid substance, solid-liquid ratio is 1 ︰ 10～30 (W/V), heating, temperature is controlled at 60～90 ℃, and extraction time is 1～5 hour, and suction filtration is removed residue and is obtained extracting solution.Repeat to extract 1～5 time, extracting solution merges.
5) sevage method is except albumen: to the sevage reagent that adds 0.1～0.3 times of volume in extracting solution, (chloroform: propyl carbinol=5 ︰ 1, V/V), stirs 20～40 minutes, and after completing, 5000 r/min centrifugal 10 minutes, get supernatant liquor.Repetitive operation 3～5 times.
6) dialysis desalting and other micromolecular compound: Deproteinated polysaccharide soln is moved in dialysis tubing, retain the space of at least 1/3 dialysis tubing system.The 24h that dialyses in the distilled water of equal volume, every 8h changes water one time, with desalination and remove other micromolecular compound.Aqueous solution concentrating under reduced pressure obtains concentrated solution.
7) polysaccharide precipitation and dry: to the ethanol that adds 3～5 times of volumes 95% in concentrated solution, hold over night, 4800 r/min, centrifugal 10 minutes, collecting precipitation.The precipitation of collecting obtains tree peony stamen Crude polysaccharides through vacuum lyophilization.
The invention provides a kind of extraction and separation process of tree peony stamen polysaccharide.The method has utilized tree peony stamen polysaccharide water-soluble and be insoluble to the character of alcohol, adopts freeze-thaw method and ultrasonication, petroleum ether degreasing, alcohol precipitation removal of impurities, and sevage method is except albumen, dialysis desalting and other micromolecular compound, and extract polysaccharide with hot water dissolving.Method is simple, controlled; Tree peony stamen polysaccharide yield can reach 3.1%, and extraction yield can reach 62.6%.
Embodiment
Embodiment 1.
1) pulverize: gather tree peony stamen, dry for 45 ℃ and pulverize, cross 40 mesh sieves.
2) cell wall breaking: the water to adding 10 times of amounts in the tree peony stamen of pulverizing, stir, be placed in Ultralow Temperature Freezer-80 ℃ freezing 14 hours.Drop in 80 ℃ of water-baths and thaw rapidly, water-bath 1 hour.Then 200W supersound process is 20 minutes, filters to such an extent that solid substance is broken wall stamen.
3) degreasing, except oligosaccharides: in the tree peony stamen after broken wall, add sherwood oil to reflux 6 hours, solid-liquid ratio is 1 ︰ 2 (W/V), and solid substance (degreasing tree peony stamen) is filtered to obtain in lixiviate degreasing.In solid substance, add 80% ethanol, solid-liquid ratio is 1 ︰ 3 (W/V), refluxes 6～8 hours, and suction filtration, to remove oligosaccharides.Repeat 1 time, suction filtration obtains solid substance (degreasing, except the tree peony stamen after oligosaccharides).
4) extraction of polysaccharide: add distilled water in solid substance, solid-liquid ratio is 1 ︰ 10～30 (W/V), heating, temperature is controlled at 60～90 ℃, and extraction time is 1～5 hour, and suction filtration is removed residue and is obtained extracting solution.Repeat to extract 1～5 time, extracting solution merges.
5) sevage method is except albumen: to the sevage reagent that adds 0.2 times of volume in supernatant liquor, (chloroform: propyl carbinol=5 ︰ 1, V/V), stirs 30 minutes, and after completing, 5000 r/min centrifugal 10 minutes, get upper water solution clear liquid.Repetitive operation 5 times, supernatant liquor merges.
6) dialysis desalting and other micromolecular compound: Deproteinated polysaccharide soln is moved in dialysis tubing, retain the space of at least 1/3 dialysis tubing system.In the distilled water of equal volume, dialyse 24 hours, within every 8 hours, change one time water, with desalination and remove other micromolecular compound.Aqueous solution concentrating under reduced pressure obtains concentrated solution.
7) polysaccharide precipitation and dry: to the ethanol that adds 4 times of volumes 95% in concentrated solution, hold over night, 4800 r/min, centrifugal 10 minutes, collecting precipitation.The precipitation of collecting obtains tree peony stamen polysaccharide through vacuum lyophilization.Tree peony polysaccharide yield is 3.1%, and extraction yield is 62.6%.
Claims (8)
1. an extraction and separation process for tree peony stamen polysaccharide, is characterized in that comprising the following steps:
1) pulverize: gather tree peony stamen, drying and crushing, sieves;
2) cell wall breaking: add water in the tree peony stamen of pulverizing, stir, be placed in Ultralow Temperature Freezer freezing; Dropping into rapidly heating in water bath in water-bath thaws; Then 200W supersound process, filters to obtain solid substance;
3) degreasing, except oligosaccharides: in the tree peony stamen after broken wall, add sherwood oil backflow lixiviate degreasing, filter to obtain solid substance; In solid substance, add 80% ethanol, reflux, suction filtration, to remove oligosaccharides; Repeat 1～3 time, suction filtration obtains solid substance, vacuum-drying;
4) extraction of polysaccharide: in solid substance, add distilled water, heating, lixiviate, suction filtration is removed residue and is obtained supernatant liquor; Repeat to extract 1～5 time, supernatant liquor merges;
5) sevage method is removed albumen: in supernatant liquor, add sevage reagent (chloroform: propyl carbinol=5:1, V/V), stir, after completing, 5000 r/min centrifugal 10 minutes, get upper water solution clear liquid;
6) dialysis desalting and other micromolecular compound: Deproteinated polysaccharide soln is moved in dialysis tubing, retain the space of at least 1/3 dialysis tubing system; The 24h that dialyses in the distilled water in equal volume, every 8h changes water one time, with desalination and remove other micromolecular compound; Aqueous solution concentrating under reduced pressure obtains concentrated solution;
7) polysaccharide precipitation and dry: the ethanol to adding 95% in concentrated solution, is placed in 0～4 ℃ and spends the night, 4800 r/min, centrifugal 10 minutes, collecting precipitation; The precipitation of collecting, through vacuum lyophilization, obtains Tree Peony flower stamen polysaccharide.
2. according in the step 1) described in right 1, it is characterized in that: after Tree Peony flower stamen dries in the shade, being crushed to particle diameter is 20～100 orders.
3. according to the step 2 described in right 1) in, it is characterized in that: the amount that adds water is 5～15 times of amounts; The temperature of Ultralow Temperature Freezer is-60～-80 ℃, and freezing time is 12～16 hours; Water-bath temperature is 70～90 ℃, and the water-bath time is 1～2 hour; The supersound process time is 10～50 minutes.
4. according in the step 3) described in right 1, it is characterized in that: in the Tree Peony flower stamen after broken wall, add sherwood oil, solid-liquid ratio is 1:2～4 (W/V), and return time is 6～8 hours; In solid substance, add 80% ethanol, solid-liquid ratio is 1:2～4 (W/V).
5. according in the step 4) described in right 1, it is characterized in that: in solid substance, add distilled water, solid-liquid ratio is 1:10～30 (W/V), and Heating temperature is 60～90 ℃, and extraction time is 1～5 hour.
6. according in the step 5) described in right 1, it is characterized in that: sevage reagent (chloroform: consumption propyl carbinol=5:1, V/V) is 0.1～0.3 times of concentrated solution volume, and churning time is 20～40 minutes; Repetitive operation 3～5 times.
7. according in the step 7) described in right 1, it is characterized in that: to the ethanol that adds 3～5 times of volumes 95% in concentrated solution.
8. according to the method described in right 1, it is characterized in that: described Varieties of Peony is Feng Dan, but be not limited to Feng Dan.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104031157A (en) * | 2014-06-03 | 2014-09-10 | 菏泽尧舜牡丹生物科技有限公司 | Method for extracting peony polysaccharide from peony seed meals |
| CN104090049A (en) * | 2014-07-07 | 2014-10-08 | 浙江大学 | Extraction method for oligosaccharide in rice seed embryos through HPLC (high performance liquid chromatography) detection |
| CN104292356A (en) * | 2014-11-11 | 2015-01-21 | 济南凯因生物科技有限公司 | Method for extracting peony polysaccharide from peony cakes with biological enzyme method |
| CN105211794A (en) * | 2015-09-10 | 2016-01-06 | 杨丽敏 | Ultralow temperature extracts the method for the pancebrin of potato activity |
| CN105440152A (en) * | 2016-01-25 | 2016-03-30 | 浙江医学高等专科学校 | Method for extracting fingered citron polysaccharide |
| CN107549807A (en) * | 2017-09-26 | 2018-01-09 | 湖南源绿科技有限公司 | The slow method for freezing combining ultrasonic ripple pretreatment high efficiency extraction active components of plants |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104031157A (en) * | 2014-06-03 | 2014-09-10 | 菏泽尧舜牡丹生物科技有限公司 | Method for extracting peony polysaccharide from peony seed meals |
| CN104090049A (en) * | 2014-07-07 | 2014-10-08 | 浙江大学 | Extraction method for oligosaccharide in rice seed embryos through HPLC (high performance liquid chromatography) detection |
| CN104090049B (en) * | 2014-07-07 | 2016-01-06 | 浙江大学 | A kind of extracting method for oligosaccharides in the rice embryo of HPLC detection |
| CN104292356A (en) * | 2014-11-11 | 2015-01-21 | 济南凯因生物科技有限公司 | Method for extracting peony polysaccharide from peony cakes with biological enzyme method |
| CN105211794A (en) * | 2015-09-10 | 2016-01-06 | 杨丽敏 | Ultralow temperature extracts the method for the pancebrin of potato activity |
| CN105440152A (en) * | 2016-01-25 | 2016-03-30 | 浙江医学高等专科学校 | Method for extracting fingered citron polysaccharide |
| CN107549807A (en) * | 2017-09-26 | 2018-01-09 | 湖南源绿科技有限公司 | The slow method for freezing combining ultrasonic ripple pretreatment high efficiency extraction active components of plants |
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Application publication date: 20140205 |