CN101456918B - Sealwort polysaccharide and preparation method thereof, and its application in preparing hypoglycemic and reducing blood lipid drugs - Google Patents
Sealwort polysaccharide and preparation method thereof, and its application in preparing hypoglycemic and reducing blood lipid drugs Download PDFInfo
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- CN101456918B CN101456918B CN2009100005339A CN200910000533A CN101456918B CN 101456918 B CN101456918 B CN 101456918B CN 2009100005339 A CN2009100005339 A CN 2009100005339A CN 200910000533 A CN200910000533 A CN 200910000533A CN 101456918 B CN101456918 B CN 101456918B
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Abstract
The invention provides a polygonatum canaliculatum polysaccharide and a preparation method thereof. The polygonatum canaliculatum polysaccharide is extracted from the perennial liliaceae herbal plant of polygonatum canaliculatum and has the molecular weight of 5,000 to 100,000 Daltons. The solid polygonatum canaliculatum polysaccharide is off white or white. The monosaccharide consists of pyrane type beta-D-galactose, D-glucose and D-mannose. The product can be developed into medicines capable of reducing blood sugar and blood fat. The preparation method is reliable and feasible, and is suitable for the volume product without environmental pollution. The preparation method has low cost.
Description
Technical field
The present invention relates to a kind of polygonatum polysaccharide, relate in particular to its preparation method and medicinal use.
Background technology
Sealwort another name celestial being surplus grain, Rhizome of Tendrilleaf Solomonseal, chicken head ginseng etc. are Liliaceae Polygonatum per nnial herbs.Smell is gentle, and quality is moistened, and the moon of tonic lung is arranged, moisturize the effect of promoting the production of body fluid.In recent years, many to the active substance of sealwort research report, as polygonatum polysaccharide hypoglycemic, delay function such as life span of drosophila melanogaster.The sealwort main component has three major types: 1. be fat-soluble steroid saponin thing; 2. be flavones, green onion quinones; 3. be water soluble component-polygonatum polysaccharide.
Sealwort is widely used in clinically, and has got better therapeutic effect for traditional Chinese medicine commonly used.Control that cough, leprosy are itched, aspect such as diabetes, cerebral arteriosclerosis dizziness, anti-ageing, reducing blood-fat has good effect.And these effects be unable to do without water soluble component-polygonatum polysaccharide.As a kind of biological activity conditioning agent, polygonatum polysaccharide has great exploitation prospect.
Chinese patent literature CN1178799A discloses a kind of extracting method of polygonatum polysaccharide, is that filtrate adds organic deposition with sealwort lower alcohol lixiviate, filtration, and throw out is through getting the polygonatum polysaccharide crude product behind the filtering drying; The polygonatum polysaccharide crude product carries out chromatography three times with weak basic anion exchange resin and polyacrylamide gel again, gets the polygonatum polysaccharide elaboration through concentrated, freeze-drying again.This preparation method's technology is loaded down with trivial details, the equipment complexity, and the treatment time is long, and yield is low, and the cost height is not suitable for industrialization production.
Chinese patent literature CN1363611A discloses a kind of extracting method of polygonatum polysaccharide, is to extract with poach earlier, and centrifugal, the supernatant liquor concentrating under reduced pressure is used the ethanol alcohol precipitation again, and the ethanol alcohol precipitation is used in the throw out washing again, throw out with washing with alcohol after, vacuum-drying is pulverized again.The polygonatum polysaccharide purity that this kind method is extracted is not high, and impurity is more, influences the medicinal effect of polygonatum polysaccharide.
Summary of the invention
First purpose of the present invention is to provide a kind of polygonatum polysaccharide.
The preparation method that provides a kind of polygonatum polysaccharide new also is provided second purpose of the present invention.
The 3rd purpose of the present invention is to provide the new medicinal use of the polygonatum polysaccharide that the present invention relates to.
The polygonatum polysaccharide that first purpose of the present invention provides, from perennial Liliaceae herbaceous plant sealwort, extract, its molecular weight is 5000～100000 dalton, solid-state being white in color to canescence, and the monose composition is mainly pyranose form β-D-semi-lactosi, D-glucose and D-seminose.
Polygonatum polysaccharide of the present invention is by following method preparation:
(1), get the sealwort medicinal material, pulverize, the sealwort powder; Get the sealwort powder, add the water that is at least 4 times of amounts of sealwort grain weight amount, heat extraction, be cooled to room temperature after extracting end, filter, get filtrate 1., the dregs of a decoction add the water heating of at least 2 times of amounts and extract, be cooled to room temperature after extracting end, filter, get filtrate 2., merge 2 times filtrate, be evaporated to 30%～60% of original filtrate volume amount, filter the filtrate for later use that obtains after the filtration;
(2), the filtrate that obtains at last in the step (1) is added the ethanol alcohol precipitation, leave standstill, centrifugal, suction filtration is got filtrate;
(3), filtrate that suction filtration in the step (2) is obtained adds the ethanol alcohol precipitation, leaves standstill, centrifugal, taking precipitate, throw out are washed 2 times with ethanol and acetone respectively, drying under reduced pressure must the polygonatum polysaccharide crude product;
(4), get the polygonatum polysaccharide crude product, add the water dissolution that is equivalent at least 10 times of amounts of polygonatum polysaccharide crude product weight, suction filtration, filtrate is with adjusting PH with base value to 9.5～13.5, and then adds quaternary ammonium salt precipitate in filtrate, leaves standstill, centrifugal, suction filtration is got filtrate;
(5), filtrate that step (4) suction filtration is obtained adds the ethanol alcohol precipitation, leaves standstill, and is centrifugal, taking precipitate;
(6), be the dissolving of 5% chloride soln with at least 3 times of throw outs that obtains in the suitable step (5) amount and mass concentration, with acid for adjusting pH value to 3.0～5.0, leave standstill, centrifugal, suction filtration is got filtrate;
(7), the filtrate that obtains to step (6) adds the ethanol alcohol precipitation, leaves standstill, throw out is washed 2 times with ethanol and acetone respectively, drying under reduced pressure must the polygonatum polysaccharide elaboration.
Quaternary ammonium salt in the described step (4) can be hexadecyl TMA (TriMethylAmine) bromide and oxyhydroxide, cetyl pyridinium, iodate N-trimethyl chitin quaternary ammonium salt or chitosan hydroxypropyl-trimethyl ammonium chloride etc.
Muriate in the described step (6) can be sodium-chlor, Repone K etc.
The acid that adjust pH described in the aforesaid method is used can be hydrochloric acid, phosphoric acid, citric acid or sulfuric acid.
The alkali that described adjust pH is used is sodium hydroxide, calcium hydroxide, potassium hydroxide, sodium bicarbonate or ammoniacal liquor.
The temperature of extracting for the first time in the described step (1) can be 85 ℃～100 ℃, and extraction time was at least 2 hours.The temperature of extracting can be 85 ℃～100 ℃ for the second time, and extraction time was at least 1 hour.
The final volume concentration of alcohol can be 10%～30% behind the middle alcohol precipitation of described step (2).
The final volume concentration of alcohol can be 40%～95% behind described step (3), (5) middle alcohol precipitation.
The application of polygonatum polysaccharide of the present invention in hypoglycemic, the blood lipid-lowering medicine of preparation also is provided.
The present invention adopts modern scientific method, described polygonatum polysaccharide is separated, purifies, and prepared polygonatum polysaccharide product safety is nontoxic, and preparation is simple, raw material is easy to get, the reaction conditions gentleness, the yield height, purity is good, environmental protection, good stability, also very low to preparation equipment and place requirement, be suitable for large-scale industrial production.
Result according to pharmacology, pharmacodynamic study shows that the prepared polygonatum polysaccharide product of the present invention has tangible effect to cardiovascular systems, can be developed into hypoglycemic, reducing blood-fat class medicine.
Embodiment
Below by specific embodiment the present invention is described in further detail, to help understanding content of the present invention.
Embodiment:
Get sealwort medicinal material 1kg, the water yield that adds 10 times of medicinal material weight is boiled extraction 3h, and suction filtration, the dregs of a decoction add 8 times water boil extraction 1h, merge 2 times filtrate, be evaporated to original filtrate volume amount 50%, suction filtration, filtrate adds 95% (v/v, down together) ethanol is to pure final concentration 20% (v/v, down together), leave standstill, supercentrifuge is centrifugal, suction filtration, filtrate adds 95% ethanol to pure final concentration 70%, leaves standstill, and is centrifugal, get precipitation, precipitation is washed 2 times with 95% ethanol and acetone respectively, and drying under reduced pressure gets polygonatum polysaccharide crude product 40.34g.
Get the polygonatum polysaccharide crude product, add the water dissolution be equivalent to 25 times of crude product weight, suction filtration, filtrate is with 40% (w%) NaOH adjust pH to 12.5, adding 5% (w%) hexadecyl TMA (TriMethylAmine) bromide solution to hexadecyl TMA (TriMethylAmine) bromide solution final concentration is 1.5% (w%) (this step has reached the effect that is further purified polygonatum polysaccharide), leave standstill, centrifugal, suction filtration, filtrate adds 95% ethanol to pure final concentration 70%, leave standstill, centrifugal, get precipitation, 5% (w%) NaCl solution dissolving with 5 times of amounts of suitable precipitation weight, with 6mol/L HCl adjust pH to 3.5 (effect of this step is to remove quaternary ammonium salt), leave standstill, centrifugal, suction filtration, filtrate adds 95% ethanol to pure final concentration 70%, leaves standstill, and is centrifugal, get precipitation, precipitation is washed 2 times with 95% ethanol and acetone respectively, and drying under reduced pressure gets polygonatum polysaccharide elaboration 4.24g.Assay is carried out in sampling, and detections such as molecular weight determination are standby.
Assay:
1. polysaccharide is differentiated: phenolsulfuric acid reagent react (positive)
2. polysaccharide content: 91.21% (measuring) with the phenolsulfuric acid method
3. polysaccharide molecule flow measurement: 37813 dalton (with reference to two appendix VH of pharmacopeia in 2005).
4. the polygonatum polysaccharide monosaccharide component is measured: record polygonatum polysaccharide and contain pyranose form β-D-semi-lactosi, D-glucose, D-seminose, and the total amount of pyranose form β-D-semi-lactosi, D-glucose, D-seminose is 88.42%.(an appendix VI of Chinese Pharmacopoeia version in 2005 D)
Experimental example
Test of pesticide effectiveness result
I, sample source: the polygonatum polysaccharide sample is pressed the self-control of embodiment method, and purity is more than 85%.
II, laboratory animal: Kunming mouse is provided by unming Medical College's Experimental Animal Center.
III, test method and result:
(1), polygonatum polysaccharide prevention effect on hyperlipemia in mice
It is some to get Kunming mouse, is divided into 6 groups at random, as table 1 and table 2.Gastric infusion is 10 days continuously, and blank group gives physiological saline, and other groups give corresponding medicine respectively.With last administration pneumoretroperitoneum injection in 1 hour egg-nog 0.5ml/25g.The physiological saline of blank group abdominal injection 0.5ml.Posterior orbit was got blood (fasting be can't help water 12 hours) in 20 hours, and 2500 rev/mins of low-temperature centrifugations are got two indexs of supernatant serum measurement TC and TG.
The effect of the hypercholesterolemia of table 1 polygonatum polysaccharide prevention mouse
Experimental result shows that dosage is that the polygonatum polysaccharide group of 0.300g/kg is suitable with the effect of Simvastatin group, so polygonatum polysaccharide has the effect of highly significant to the hypercholesterolemia to the prevention mouse.
The effect of table 2 polygonatum polysaccharide prevention mouse triglyceride
Experimental result shows that dosage is that the polygonatum polysaccharide group of 0.300g/kg is suitable with the effect of Simvastatin group, so polygonatum polysaccharide has the effect of highly significant to the triglyceride to the prevention mouse.
(2), polygonatum polysaccharide reduces the effect of mouse blood sugar.
It is some to get male mice in kunming, is divided into 8 groups at random.Test preceding mouse fasting after 12 hours, the tetraoxypyrimidine of tail vein injection 70mg/kg.Tail vein injection 5.0% glucose 0.4ml after 4 hours.Treated to survey blood glucose value when blood sugar rises to the peak period in the 3rd day of experiment, the mouse that selects blood glucose value＞16.6mmol/l is as the administration object.Each group is irritated stomach and is given corresponding medicine, and once a day, positive drug sooner or later respectively is administered once successive administration seven days.The blood glucose value of respectively organizing experiment mice is surveyed in the last administration after 2 hours.
Table 3 polygonatum polysaccharide reduces the effect of mouse blood sugar
Compare P＜0.01 with the blank group
Experimental result shows that model and blank relatively have significant difference (P＜0.01).On each administration group and the model group comparative statistics significant difference is arranged, wherein polygonatum polysaccharide group blood sugar decreasing effect 3. is best.Test-results shows that polygonatum polysaccharide has the effect of significant reduction mouse blood sugar.
Claims (10)
1. polygonatum polysaccharide, from perennial Liliaceae herbaceous plant sealwort, extract, it is characterized in that: its molecular weight is 5000～100000 dalton, solid-state being white in color to canescence, and the monose composition is mainly pyranose form β-D-semi-lactosi, D-glucose and D-seminose.
2. the preparation method of a polygonatum polysaccharide comprises following process successively:
(1), get the sealwort medicinal material, pulverize, the sealwort powder; Get the sealwort powder, add the water of the 4 times of amounts of weight that are at least the sealwort powder, heat and extract, extraction is cooled to room temperature after finishing, and filters, and gets filtrate; The water that the dregs of a decoction add at least 2 times of amounts heats extraction, and extraction is cooled to room temperature after finishing, and filters, and gets filtrate; Merge 2 times filtrate, be evaporated to 30%～60% of original filtrate volume amount, filter the filtrate for later use that obtains after the filtration;
(2), the filtrate that obtains at last in the step (1) is added the ethanol alcohol precipitation, leave standstill, centrifugal, suction filtration is got filtrate;
(3), filtrate that suction filtration in the step (2) is obtained adds the ethanol alcohol precipitation, leaves standstill, centrifugal, taking precipitate, throw out are washed 2 times with ethanol and acetone respectively, drying under reduced pressure must the polygonatum polysaccharide crude product;
(4), get the polygonatum polysaccharide crude product, add the water dissolution that is equivalent at least 10 times of amounts of polygonatum polysaccharide crude product weight, suction filtration, filtrate is with adjusting PH with base value to 9.5～13.5, and then adds quaternary ammonium salt precipitate in filtrate, leaves standstill, centrifugal, suction filtration is got filtrate;
(5), filtrate that step (4) suction filtration is obtained adds the ethanol alcohol precipitation, leaves standstill, and is centrifugal, taking precipitate;
(6), be 5% chloride soln dissolving with at least 3 times of weight of precipitate that obtain in the suitable step (5) and mass concentration, with acid for adjusting pH value to 3.0～5.0, leave standstill, centrifugal, suction filtration is got filtrate;
(7), the filtrate that obtains to step (6) adds the ethanol alcohol precipitation, leaves standstill, and isolates throw out and washes 2 times with ethanol and acetone respectively, drying under reduced pressure must the polygonatum polysaccharide elaboration.
3. preparation method as claimed in claim 2 is characterized in that: the quaternary ammonium salt in the described step (4) is hexadecyl TMA (TriMethylAmine) bromide and oxyhydroxide, cetyl pyridinium, iodate N-trimethyl chitin quaternary ammonium salt or chitosan hydroxypropyl-trimethyl ammonium chloride.
4. as claim 2 or 3 described preparation methods, it is characterized in that: the muriate in the described step (6) is sodium-chlor or Repone K.
5. as claim 2 or 3 described preparation methods, it is characterized in that: the acid that described adjust pH is used is hydrochloric acid, phosphoric acid, citric acid or sulfuric acid.
6. as claim 2 or 3 described preparation methods, it is characterized in that: the alkali that described adjust pH is used is sodium hydroxide, calcium hydroxide, potassium hydroxide, sodium bicarbonate or ammoniacal liquor.
7. as claim 2 or 3 described preparation methods, it is characterized in that: the temperature of extracting for the first time in the described step (1) is 85 ℃～100 ℃, and extraction time was at least 2 hours; The temperature of extracting is 85 ℃～100 ℃ for the second time, and extraction time was at least 1 hour.
8. as claim 2 or 3 described preparation methods, it is characterized in that: the final volume concentration of alcohol is 10%～30% behind the middle alcohol precipitation of described step (2).
9. as claim 2 or 3 described preparation methods, it is characterized in that: the final volume concentration of alcohol is 40%～95% behind described step (3), (5) middle alcohol precipitation.
10. the application in the described polygonatum polysaccharide of claim 1, the blood lipid-lowering medicine hypoglycemic in preparation.
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| CN2009100005339A CN101456918B (en) | 2009-01-16 | 2009-01-16 | Sealwort polysaccharide and preparation method thereof, and its application in preparing hypoglycemic and reducing blood lipid drugs |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102351961A (en) * | 2011-11-15 | 2012-02-15 | 重庆市秀山红星中药材开发有限公司 | Method for extracting rhizoma polygonati polysaccharide from stems and leaves of rhizoma polygonati |
| CN102351960B (en) * | 2011-11-15 | 2013-07-10 | 重庆市秀山红星中药材开发有限公司 | Method for extracting rhizoma polygonati polysaccharide |
| CN102491999A (en) * | 2011-11-15 | 2012-06-13 | 重庆市秀山红星中药材开发有限公司 | Method for extracting polygonatum rhizome oligosaccharide |
| CN105218692B (en) * | 2014-06-05 | 2018-01-30 | 上海家化联合股份有限公司 | A kind of sealwort β galactans and preparation method thereof and the application for suppressing Apoptosis |
| CN107586343A (en) * | 2016-07-08 | 2018-01-16 | 玉溪众欣农业科技有限公司 | A kind of Siberian solomonseal rhizome polysaccharide extraction process |
| CN107259429A (en) * | 2017-06-18 | 2017-10-20 | 合肥睿联生物科技有限公司 | A kind of wonderful taste longan of Siberian solomonseal rhizome polysaccharide and preparation method thereof |
| CN107279917A (en) * | 2017-06-18 | 2017-10-24 | 合肥睿联生物科技有限公司 | A kind of tasty bar denier wood of Siberian solomonseal rhizome polysaccharide and preparation method thereof |
| CN107319464A (en) * | 2017-06-18 | 2017-11-07 | 合肥睿联生物科技有限公司 | A kind of wonderful taste Chinese chestnut of Siberian solomonseal rhizome polysaccharide and preparation method thereof |
| CN107242511A (en) * | 2017-06-18 | 2017-10-13 | 合肥睿联生物科技有限公司 | A kind of tasty melon seeds of Siberian solomonseal rhizome polysaccharide and preparation method thereof |
| CN110845639A (en) * | 2019-12-31 | 2020-02-28 | 山东省分析测试中心 | Method for extracting polygonatum polysaccharide |
| CN113004433A (en) * | 2021-03-09 | 2021-06-22 | 成都中医药大学 | Rhizoma polygonati fructan and preparation method and application thereof |
Citations (2)
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| CN1796418A (en) * | 2004-12-30 | 2006-07-05 | 中国科学院上海药物研究所 | Immune polysaccharide of rhizome of manyflower solomonseal, composition and application |
| CN101255199A (en) * | 2008-03-25 | 2008-09-03 | 西安交通大学 | A method for extracting Polygonatum Polysaccharide from Rhizoma Polygonatum |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1796418A (en) * | 2004-12-30 | 2006-07-05 | 中国科学院上海药物研究所 | Immune polysaccharide of rhizome of manyflower solomonseal, composition and application |
| CN101255199A (en) * | 2008-03-25 | 2008-09-03 | 西安交通大学 | A method for extracting Polygonatum Polysaccharide from Rhizoma Polygonatum |
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