CN101450972A - Ethanol concentration gradient technique for lily polysaccharide purification - Google Patents
Ethanol concentration gradient technique for lily polysaccharide purification Download PDFInfo
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- CN101450972A CN101450972A CNA2007101715393A CN200710171539A CN101450972A CN 101450972 A CN101450972 A CN 101450972A CN A2007101715393 A CNA2007101715393 A CN A2007101715393A CN 200710171539 A CN200710171539 A CN 200710171539A CN 101450972 A CN101450972 A CN 101450972A
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Abstract
The invention provides a lily polysaccharide purification process applicable to industrial production, namely a novel process for purifying lily polysaccharide through ethanol concentration gradient. The process comprises the steps of subjecting a lily polysaccharide concentrated solution to alcohol precipitation and protein removal once, utilizing ethanol solution with the concentration gradient between 75 and 95 percent to cyclically wash the concentrated solution 2 to 5 times and obtaining a pure lily polysaccharide product with the purity more than 70 percent. Meanwhile, the yield of lily polysaccharide is more than 68 percent of the lily polysaccharide content of lily. In addition, as the use frequency and use amount of chloroform are reduced, more than 80 percent of chloroform residue in the lily polysaccharide can be reduced. The process has the advantages of simple efficient flow, economical efficiency, environmental protection and suitability for industrial production and application.
Description
Technical field
The present invention relates to a kind of lily polysaccharide process for extracting, especially a kind of purifying process that is applicable to the lily polysaccharide of suitability for industrialized production.
Background technology
Quote the Chinese medicine in more than 2,000 year as a kind of traditional Chinese medical science, lily has clearly, significant curative effect (referring to the record in " Dragon Lord book on Chinese herbal medicine through ", " not Lu " and the Holy Benevolent Prescriptions).Lily herbal function characteristics show mainly that i.e. replenishing YIN and removing heat, moistening lung are quenched the thirst in " nourishing with health care ", the effect of tranquillizing by calming the heart and invigorating the spleen and replenishing QI.Functional and the economic worth that lily polysaccharide has in lily effective constituent, it functional mainly comprises effect that good enhancing immunity regulates, antitumor activity, anti-oxidant, strengthening by means of tonics and anti-aging effects and obvious functions of blood sugar function, and the percentage composition of lily polysaccharide in lily is in the front three of lily component content.Lily polysaccharide extracts and can be nourishing of Development and Production lily polysaccharide and healthcare product, and exploitation polysaccharide newtype drug is supplied raw materials.
What the lixiviate that existing laboratory is used, ethanol sedimentation, Deproteinated lily polysaccharide extraction process generally obtained is the lily Crude polysaccharides, and to obtain purer lily polysaccharide, normally adopt two kinds of processing methodes at present: the one, the method by chromatography column under lab, this method extracted amount is little, production efficiency is low, and the lily polysaccharide loss amount is big, and polysaccharide yield is not high, is difficult to be applied in the industrial production; The 2nd, utilize propyl carbinol/chloroform mixed solution to purify, but this method chloroform consumption is big by 3-5 circulation (Svage method), residual quantity is big, and strong toxicity is seriously polluted, and cost is also high, and purification efficiency is low, and is unfavorable to suitability for industrialized production.
Find by prior art documents, do not extract relevant patent documentation report both at home and abroad at present with lily polysaccharide, in non-patent literature, lily polysaccharide extraction process pertinent literature report is arranged, method (Liu Chengmei, Fu Guiming etc., the purifying of lily polysaccharide and chemical structure identification research as chromatography column, Food science, 114) and Svage method (Liu Chengmei, Wan Yin etc. 2002,23 (5):, the research of lily polysaccharide method for removing protein, Food science, 2002,23 (1): 89), but the relevant report that does not still have the ethanol concentration gradient technique of lily polysaccharide purification does not have the report that lily polysaccharide extracts the industrialization aspect yet.
Summary of the invention
Above-mentioned deficiency at the lily polysaccharide purification Technology, the invention provides a kind of purifying process that is applicable to the lily polysaccharide of suitability for industrialized production, it is ethanol concentration gradient purifying lily polysaccharide novel process, it is in the purity and yield that guarantee lily polysaccharide, reduce the consumption of chloroform, thereby reduce the pollution of toxic solvents, reduce production costs, industrial suitability is provided.The present invention is the novel process of the highly purified lily polysaccharide of high efficiency extraction.
The present invention is achieved by the following technical solutions, the present invention the lily polysaccharide concentrated solution through alcohol precipitation, Deproteinization once after, utilize ethanolic soln circulation cleaning 2-5 time of 75%-95% concentration gradient, make highly purified lily polysaccharide.The purpose of taking repeatedly to wash is sex change and removes proteolytic enzyme, amino acid impurity, and the ethanol of lower concentration can be taken away the oligosaccharides of most of small molecular weight simultaneously, and ethanol concentration gradient purifying multiple number of times is many more, and product is pure more high more, but polysaccharide loss is big more.
Utilize ethanol concentration gradient purifying of the present invention, the lily polysaccharide pure product of purity greater than 70% can obtained, the lily polysaccharide yield be in the lily lily polysaccharide content 80%, can reduce simultaneously in the lily polysaccharide chloroform residual quantity more than 65%, technical process is simple efficient, economical and be beneficial to environmental protection.
Embodiment
Below in conjunction with example in detail the present invention.
Embodiment one:
With new fresh Bulbus Lilii bulb, dry back baking about 60 ℃ naturally and smash sieving for standby then to absolutely dry.Take by weighing lily bulb powder through 85% ethanol about 10h of backflow under 80 ℃, filter.Filter residue filters with 55 ℃ of following lixiviate 5h of deionized water, gets lily polysaccharide vat liquor crude product.
The lily polysaccharide vat liquor behind concentrating under reduced pressure with 90% long-pending ethanol sedimentation of tetraploid, crossing the leaching precipitation back that is dissolved in water adopts Svage method Deproteinization once (the Svage method is for adding equal-volume chloroform/propyl carbinol mixed solution, the volume ratio 5:2 of chloroform/propyl carbinol in the mixed solution, fully vibration), post precipitation is got supernatant liquor, obtains rough lily polysaccharide solution.Adopt thick lily polysaccharide saturated solution to add the further enzymolysis protein of proteolytic enzyme, then with the long-pending ethanol sedimentation of tetraploid.Get precipitation respectively with 75% ethanol, the washing of 85% and 95% straight alcohol and repeat (gradient ethanolic soln washing method) 2 times, acetone is used in last circulation, and washing with alcohol precipitates and obtains the lily polysaccharide essence after the drying and carry product.
The pure product of lily polysaccharide that routine thus ethanol concentration gradient purifying prepares for 2 times, its purity is more than 75%, the lily polysaccharide yield be in the lily lily polysaccharide content 86%, it is about 80% to reduce in the lily polysaccharide chloroform residual quantity simultaneously, has that technical process is simple, technological advantages such as economy and environmental protection.
Embodiment two:
New fresh Bulbus Lilii bulb is cleaned, and 20 kilograms of gauze bag packings drop into 200 liters extractor, with 95 ℃ of following lixiviate 2h of deionized water, shift extracting solution then to concentration tank.Add deionized water in the extractor, repeat to extract 2 times, shift extracting solution to concentration tank.No. 3 extracting solutions are vacuumized concentrated in concentration tank under 90 ℃, are concentrated into 30% discharging, lily polysaccharide medicinal extract crude product.
Lily polysaccharide medicinal extract is with 95% long-pending ethanol sedimentation of tetraploid, crossing the leaching precipitation back that is dissolved in water adopts Svage method Deproteinization once (the Svage method is for adding equal-volume chloroform/propyl carbinol mixed solution, the volume ratio 5:2 of chloroform/propyl carbinol in the mixed solution, fully vibration), post precipitation is got supernatant liquor, obtains rough lily polysaccharide solution.Adopt thick lily polysaccharide saturated solution to add the further enzymolysis protein of proteolytic enzyme, and amass ethanol sedimentation with tetraploid.Get precipitation respectively with 85% ethanol and 95% above straight alcohol washing and repeat (gradient ethanolic soln washing method) 3 times, acetone is used in last circulation, and washing with alcohol precipitates and obtains the lily polysaccharide essence after the drying and carry product.
The pure product of lily polysaccharide that routine thus ethanol concentration gradient purifying prepares for 3 times, its purity is more than 85%, the lily polysaccharide yield be in the lily lily polysaccharide content 81%, it is about 90% to reduce in the lily polysaccharide chloroform residual quantity simultaneously, has that technical process is simple, yield is moderate and technological advantage such as environmental protection.
Embodiment three:
Lily bulb dry plate is packed with gauze bag for 15 kilograms, dropped into 200 liters extractor,, shift extracting solution then to concentration tank with 95 ℃ of following lixiviate 2h of deionized water.Add deionized water in the extractor, repeat to extract 3 times, shift extracting solution to concentration tank.No. 4 extracting solutions are vacuumized concentrated in concentration tank under 90 ℃, are concentrated into 30% discharging, lily polysaccharide medicinal extract crude product.
Lily polysaccharide medicinal extract is with 95% long-pending ethanol sedimentation of tetraploid, crossing the leaching precipitation back that is dissolved in water adopts Svage method Deproteinization once (the Svage method is for adding equal-volume chloroform/propyl carbinol mixed solution, the volume ratio 5:2 of chloroform/propyl carbinol in the mixed solution, fully vibration), post precipitation is got supernatant liquor, obtains rough lily polysaccharide solution.Adopt thick lily polysaccharide saturated solution to add the further enzymolysis protein of proteolytic enzyme, and amass ethanol sedimentation with tetraploid.Get precipitation respectively with 80% ethanol and 90% above straight alcohol washing and repeat (gradient ethanolic soln washing method) 5 times, acetone is used in last circulation, and washing with alcohol precipitates and obtains the lily polysaccharide essence after the drying and carry product.
The pure product of lily polysaccharide that routine thus ethanol concentration gradient purifying prepares for 2 times, its purity is 95%, the lily polysaccharide yield be in the lily lily polysaccharide content 68%, reduce chloroform residual quantity about 96% in the lily polysaccharide simultaneously, have technological advantages such as the simple and environmental protection of technical process, but yield is lower.
Claims (3)
1. the present invention relates to a kind of lily polysaccharide process for extracting, especially a kind of purifying process that is applicable to the lily polysaccharide of suitability for industrialized production.The ethanol concentration gradient technique that it is characterized in that lily polysaccharide purification, promptly the lily polysaccharide concentrated solution through alcohol precipitation, Deproteinization once after, utilize ethanolic soln circulation cleaning 2-5 time of 75%-95% concentration gradient, make purity greater than 70% pure product of lily polysaccharide, the lily polysaccharide yield is more than 68% of lily polysaccharide content in the lily simultaneously, simultaneously owing to reduced the access times and the usage quantity of chloroform, thereby can reduce in the lily polysaccharide chloroform residual quantity more than 80%.
2. the ethanol concentration gradient technique of lily polysaccharide purification as claimed in claim 1, it is characterized in that described lily polysaccharide concentrated solution, can by fresh Bulbus Lilii ball bulb, dried lily bulb the water extracting liquid acquisition of raw material, and the merging concentrated solution of multiple extraction liquid, its extractor can be the extractor of technical grade;
3. the ethanol concentration gradient technique of lily polysaccharide purification as claimed in claim 1, it is characterized in that described Deproteinization is the Svage method, promptly concentrate and add equal-volume chloroform/propyl carbinol mixed solution in the precipitation solution at polysaccharide, the volume ratio 5:2 of chloroform/propyl carbinol in the mixed solution, fully vibration, repeated multiple times is to remove albumen impurity.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007101715393A CN101450972A (en) | 2007-11-30 | 2007-11-30 | Ethanol concentration gradient technique for lily polysaccharide purification |
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| CNA2007101715393A CN101450972A (en) | 2007-11-30 | 2007-11-30 | Ethanol concentration gradient technique for lily polysaccharide purification |
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| CN101450972A true CN101450972A (en) | 2009-06-10 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911288A (en) * | 2012-10-23 | 2013-02-06 | 陕西科技大学 | Method for decolouring and purifying pectin |
| CN110551232A (en) * | 2019-09-25 | 2019-12-10 | 河南城建学院 | Extraction method of medicinal and edible dual-purpose lily polysaccharide and application of medicinal and edible dual-purpose lily polysaccharide in health care products |
| CN111607012A (en) * | 2020-05-29 | 2020-09-01 | 西南林业大学 | Paeonia suffruticosa polysaccharide extract and preparation method and application thereof |
| CN113425739A (en) * | 2021-08-03 | 2021-09-24 | 湖南中医药大学第一附属医院((中医临床研究所)) | Lily and rehmannia compound polysaccharide with anxiolytic and antidepressant effects and application thereof |
-
2007
- 2007-11-30 CN CNA2007101715393A patent/CN101450972A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102911288A (en) * | 2012-10-23 | 2013-02-06 | 陕西科技大学 | Method for decolouring and purifying pectin |
| CN102911288B (en) * | 2012-10-23 | 2014-12-10 | 陕西科技大学 | Method for decolouring and purifying pectin |
| CN110551232A (en) * | 2019-09-25 | 2019-12-10 | 河南城建学院 | Extraction method of medicinal and edible dual-purpose lily polysaccharide and application of medicinal and edible dual-purpose lily polysaccharide in health care products |
| CN111607012A (en) * | 2020-05-29 | 2020-09-01 | 西南林业大学 | Paeonia suffruticosa polysaccharide extract and preparation method and application thereof |
| CN113425739A (en) * | 2021-08-03 | 2021-09-24 | 湖南中医药大学第一附属医院((中医临床研究所)) | Lily and rehmannia compound polysaccharide with anxiolytic and antidepressant effects and application thereof |
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Open date: 20090610 |