CN103641926A - Extraction method of Chinese hawthorn leaf polysaccharide - Google Patents
Extraction method of Chinese hawthorn leaf polysaccharide Download PDFInfo
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- CN103641926A CN103641926A CN201310642028.0A CN201310642028A CN103641926A CN 103641926 A CN103641926 A CN 103641926A CN 201310642028 A CN201310642028 A CN 201310642028A CN 103641926 A CN103641926 A CN 103641926A
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Abstract
The invention discloses an extraction method of Chinese hawthorn leaf polysaccharide. The method, which is used for ultrasonic-assisted extraction of Chinese hawthorn leaf polysaccharide, comprises the following steps: with Chinese hawthorn leaf powder after flavone is extracted as a raw material, adding water; carrying out ultrasonic treatment; centrifugalizing; reserving supernate; concentrating under reduced pressure; settling by ethanol; standing, centrifugalizing and dissolving precipitates by water; adding chloroform-n-butyl alcohol mixed liquor; centrifugalizing; reserving supernate; concentrating under reduced pressure; adding ethanol; and standing, centrifugalizing, taking precipitate, and drying to obtain Chinese hawthorn leaf polysaccharide. The method disclosed by the invention is simple in operation, short in extraction time and less in energy consumption, is particularly suitable for industrialized production of manufacturers for preparing Chinese hawthorn leaf flavone, and is few in investment and high in profit. The method can effectively extract Chinese hawthorn leaf polysaccharide with stronger oxidation resistance.
Description
Technical field
The present invention relates to a kind of method that adopts ultrasonic-assisted extraction Howthorn Leaf polysaccharide, belong to processing of agriculture product field.
Background technology
Howthorn Leaf is the dry leave of rosaceous plant Fruit of Pashi Pear (Crataegus pinnatifida Bunge Var.major N.E.Br) or hawthorn (Crataegus pinnatifida Bge.).Its taste acid, property are put down, and return Liver Channel, have effect promoting blood circulation and removing blood stasis, that regulate the flow of vital energy and promote blood circulation, by < < Chinese Pharmacopoeia > > (2005 editions), are recorded.At present, extraction and activity research about crataegutt are more, and be widely used in clinically, such as take the preparations such as beneficial heart sheet that crataegutt is main component, capsule, dripping pill, by < < Pharmacopoeia of People's Republic of China > >, recorded.
Polysaccharide has effects such as regulating immunity of organisms, antitumor, anti-oxidant, hypoglycemic, reducing blood-fat, is a kind of important functional additive of protective foods.At present, seldom, and the Howthorn Leaf powder that extracted flavones contains abundant polysaccharide, is all taken as refuse and processes in the research of relevant Howthorn Leaf polysaccharide.In order to turn waste into wealth, improve resource utilization, the Howthorn Leaf powder that extracted flavones of take is raw material, the extractive technique of exploitation Howthorn Leaf polysaccharide has great importance.At present, have no the report that extracted polysaccharide from extracted the Howthorn Leaf powder of flavones.
Summary of the invention
The object of this invention is to provide a kind of preparation method who extracted Howthorn Leaf polysaccharide from extracted the Howthorn Leaf powder of flavones with ultrasonic wave auxiliary law.The method technique is simple, workable, effectively shortens extraction time, reduces costs, and has improved Howthorn Leaf resource utilization and added value thereof.
The object of the invention is to be achieved by following technical proposals:
An extracting method for Howthorn Leaf polysaccharide, the method comprises the following steps:
A, the Howthorn Leaf powder that extracted flavones of take are raw material, according to Howthorn Leaf powder, be 1 with the ratio of quality: 10-40 feeds intake, ultrasonication 0.2-2 hour, centrifugation, supernatant liquor is Howthorn Leaf polysaccharide extraction liquid, throw out is Howthorn Leaf residue, leave and take supernatant liquor, obtain and extract for the first time polysaccharide liquid, throw out adds water, amount of water amount of water when extracting is for the first time identical, ultrasonication 0.2-2 hour, centrifugal, leave and take supernatant liquor, obtain and extract for the second time polysaccharide liquid, merge and extract for the first time and for the second time polysaccharide liquid;
B, by polysaccharide liquid concentrating under reduced pressure to the long-pending 1/3-1/4 of polysaccharide liquid, obtain concentrated solution, under agitation condition, to adding concentrated solution volume 4-5 ethanol doubly in concentrated solution, be cooled to 0-4 ℃, standing 10-15 hour, centrifugal, throw out is Howthorn Leaf polysaccharide crude;
C, get Howthorn Leaf polysaccharide crude, adding water dissolves completely, add successively chloroform and propyl carbinol, polysaccharide soln: chloroform: the volume ratio of propyl carbinol is 15: 4: 1, keep turn/hour vibration of 100-300 centrifugal after 0.2-0.5 hour, get supernatant liquor, repetitive operation several, until supernatant liquor is collected in sediment-free appearance, the 1/3-1/4 that is concentrated to supernatant liquor volume, obtains concentrated solution;
D, under agitation condition, to adding concentrated solution volume 4-5 ethanol doubly in concentrated solution, be cooled to 0-4 ℃, centrifugal after standing 10-15 hour, collecting precipitation thing, in 50 ℃ dry, obtain Howthorn Leaf polysaccharide.
The described order number that extracted the Howthorn Leaf powder of flavones is 12-8 order.
The described Howthorn Leaf powder that extracted flavones is after Howthorn Leaf is pulverized, sieved, and first uses sherwood oil in 50 ℃ of processing 1-2 hour, filters, and adds 60-80% ethanol in filter residue, and ultrasonication, filters, and filter residue is drying to obtain at 50 ℃ the Howthorn Leaf powder that extracted flavones.
In described step b, concentrating under reduced pressure condition is 50-60 ℃, vacuum tightness < 0.1MPa.
The Howthorn Leaf polysaccharide that the above-mentioned preparation method of the present invention makes has certain anti-oxidant activity.When Howthorn Leaf polysaccharide concentration is 2mg/ml, to the clearance rate of 1,1-phenylbenzene-2-trinitrophenyl-hydrazine, can reach 59.67-63.55%.
Advantage of the present invention and positively effect are:
1, to take the Howthorn Leaf powder that extracted flavones be raw material to preparation method of the present invention, adopt ultrasonic wave auxiliary law to prepare Howthorn Leaf polysaccharide, the method is simple to operate, effectively shorten extraction time, energy consumption is little, and cost is low, and the producer that is especially applicable to preparing crataegutt carries out suitability for industrialized production, not only less investment, and profit is high.
3, the prepared Howthorn Leaf polysaccharide anti-oxidant activity of preparation method of the present invention is stronger.
Embodiment
Below in conjunction with embodiment, the invention will be further described.
Embodiment 1:
A, take the Howthorn Leaf powder that 5g extracted flavones, add water, the mass ratio of water and Howthorn Leaf powder is 30: 1, ultrasonication 0.4 hour, centrifugation, supernatant liquor is Howthorn Leaf polysaccharide extraction liquid, throw out is Howthorn Leaf residue, leaves and takes supernatant liquor, obtains and extracts for the first time polysaccharide liquid, throw out adds water, and amount of water amount of water when extracting is for the first time identical, ultrasonication 0.4 hour, centrifugal, leave and take supernatant liquor, obtain and extract for the second time polysaccharide liquid, merge and extract for the first time and for the second time polysaccharide liquid;
B, by polysaccharide liquid concentrating under reduced pressure to polysaccharide liquid long-pending 1/4, obtain concentrated solution, under agitation condition, the ethanol to adding 4 times of concentrated solution volumes in concentrated solution, is cooled to 0-4 ℃, centrifugal after standing 10 hours, throw out is Howthorn Leaf polysaccharide crude;
C, get Howthorn Leaf polysaccharide crude, adding water dissolves completely, add successively chloroform and propyl carbinol, polysaccharide soln: chloroform: the volume ratio of propyl carbinol is 15: 4: 1, keep 100 turn/hour vibrations centrifugal after 0.25 hour, get supernatant liquor, repetitive operation several, until supernatant liquor is collected in sediment-free appearance, be concentrated to 1/4 of supernatant liquor volume, obtain concentrated solution;
D, under agitation condition, the ethanol to adding 4 times of concentrated solution volumes in concentrated solution, is cooled to 0-4 ℃, centrifugal after standing 10 hours, collecting precipitation thing, in 50 ℃ dry, obtain Howthorn Leaf polysaccharide.
The extraction yield of Howthorn Leaf polysaccharide is 1.26%; When take Howthorn Leaf polysaccharide concentration that aforesaid method obtains during as 2mg/mL, to the clearance rate of 1,1-phenylbenzene-2-trinitrophenyl-hydrazine, be 63.55%.
Embodiment 2:
A, take the Howthorn Leaf powder that 5g extracted flavones, add water, the mass ratio of water and Howthorn Leaf powder is 25: 1, ultrasonication 0.4 hour, centrifugation, supernatant liquor is Howthorn Leaf polysaccharide extraction liquid, throw out is Howthorn Leaf residue, leaves and takes supernatant liquor, obtains and extracts for the first time polysaccharide liquid, throw out adds water, and amount of water amount of water when extracting is for the first time identical, ultrasonication 0.4 hour, centrifugal, leave and take supernatant liquor, obtain and extract for the second time polysaccharide liquid, merge and extract for the first time and for the second time polysaccharide liquid;
B, by polysaccharide liquid concentrating under reduced pressure to polysaccharide liquid long-pending 1/4, obtain concentrated solution, under agitation condition, the ethanol to adding 4 times of concentrated solution volumes in concentrated solution, is cooled to 0-4 ℃, centrifugal after standing 12 hours, throw out is Howthorn Leaf polysaccharide crude;
C, get Howthorn Leaf polysaccharide crude, adding water dissolves completely, add successively chloroform and propyl carbinol, polysaccharide soln: chloroform: the volume ratio of propyl carbinol is 15: 4: 1, keep 300 turn/hour vibrations centrifugal after 0.33 hour, get supernatant liquor, repetitive operation several, until supernatant liquor is collected in sediment-free appearance, be concentrated to 1/3 of supernatant liquor volume, obtain concentrated solution;
D, under agitation condition, the ethanol to adding 5 times of concentrated solution volumes in concentrated solution, is cooled to 0-4 ℃, centrifugal after standing 12 hours, collecting precipitation thing, in 50 ℃ dry, obtain Howthorn Leaf polysaccharide.
The extraction yield of Howthorn Leaf polysaccharide is 2.16%; When take Howthorn Leaf polysaccharide concentration that aforesaid method obtains during as 2mg/mL, to the clearance rate of 1,1-phenylbenzene-2-trinitrophenyl-hydrazine, be 62.12%.
Embodiment 3:
A, take the Howthorn Leaf powder that 5g extracted flavones, add water, the mass ratio of water and Howthorn Leaf powder is 35: 1, ultrasonication 0.3 hour, centrifugation, supernatant liquor is Howthorn Leaf polysaccharide extraction liquid, throw out is Howthorn Leaf residue, leaves and takes supernatant liquor, obtains and extracts for the first time polysaccharide liquid, throw out adds water, and amount of water amount of water when extracting is for the first time identical, ultrasonication 0.3 hour, centrifugal, leave and take supernatant liquor, obtain and extract for the second time polysaccharide liquid, merge and extract for the first time and for the second time polysaccharide liquid;
B, by polysaccharide liquid concentrating under reduced pressure to polysaccharide liquid long-pending 1/4, obtain concentrated solution, under agitation condition, the ethanol to adding 4 times of concentrated solution volumes in concentrated solution, is cooled to 0-4 ℃, centrifugal after standing 11 hours, throw out is Howthorn Leaf polysaccharide crude;
C, get Howthorn Leaf polysaccharide crude, adding water dissolves completely, add successively chloroform and propyl carbinol, polysaccharide soln: chloroform: the volume ratio of propyl carbinol is 15: 4: 1, keep 200 turn/hour vibrations centrifugal after 0.25 hour, get supernatant liquor, repetitive operation several, until supernatant liquor is collected in sediment-free appearance, be concentrated to 1/4 of supernatant liquor volume, obtain concentrated solution;
D, under agitation condition, the ethanol to adding 4 times of concentrated solution volumes in concentrated solution, is cooled to 0-4 ℃, centrifugal after standing 11 hours, collecting precipitation thing, in 50 ℃ dry, obtain Howthorn Leaf polysaccharide.
The extraction yield of Howthorn Leaf polysaccharide is 1.73%; When take Howthorn Leaf polysaccharide concentration that aforesaid method obtains during as 2mg/mL, to the clearance rate of 1,1-phenylbenzene-2-trinitrophenyl-hydrazine, be 62.25%.
Claims (4)
1. an extracting method for Howthorn Leaf polysaccharide, is characterized in that comprising the steps:
A, the Howthorn Leaf powder that extracted flavones of take are raw material, according to Howthorn Leaf powder, be 1 with the ratio of quality: 10-40 feeds intake, ultrasonication 0.2-2 hour, centrifugation, supernatant liquor is Howthorn Leaf polysaccharide extraction liquid, throw out is Howthorn Leaf residue, leave and take supernatant liquor, obtain and extract for the first time polysaccharide liquid, throw out adds water, amount of water amount of water when extracting is for the first time identical, ultrasonication 0.2-2 hour, centrifugal, leave and take supernatant liquor, obtain and extract for the second time polysaccharide liquid, merge and extract for the first time and for the second time polysaccharide liquid;
B, by polysaccharide liquid concentrating under reduced pressure to the long-pending 1/3-1/4 of polysaccharide liquid, obtain concentrated solution, under agitation condition, to adding concentrated solution volume 4-5 ethanol doubly in concentrated solution, be cooled to 0-4 ℃, centrifugal after standing 10-15 hour, throw out is Howthorn Leaf polysaccharide crude;
C, get Howthorn Leaf polysaccharide crude, adding water dissolves completely, add successively chloroform and propyl carbinol, polysaccharide soln: chloroform: the volume ratio of propyl carbinol is 15: 4: 1, keep turn/hour vibration of 100-300 centrifugal after 0.2-0.5 hour, get supernatant liquor, repetitive operation several, until supernatant liquor is collected in sediment-free appearance, the 1/3-1/4 that is concentrated to supernatant liquor volume, obtains concentrated solution;
D, under agitation condition, to adding concentrated solution volume 4-5 ethanol doubly in concentrated solution, be cooled to 0-4 ℃, centrifugal after standing 10-15 hour, collecting precipitation thing, in 50 ℃ dry, obtain Howthorn Leaf polysaccharide.
2. the extracting method of Howthorn Leaf polysaccharide according to claim 1, the order number that it is characterized in that extracting described in step a the Howthorn Leaf powder of flavones is 12-8 order.
3. the extracting method of Howthorn Leaf polysaccharide according to claim 1, the Howthorn Leaf powder that it is characterized in that extracting described in step a flavones is after Howthorn Leaf is pulverized, sieved, first with sherwood oil, in 50 ℃, process 1-2 hour, filter, in filter residue, add 60-80% ethanol, ultrasonication, filters, and filter residue is drying to obtain at 50 ℃ the Howthorn Leaf powder that extracted flavones.
4. the extracting method of Howthorn Leaf polysaccharide according to claim 1, is characterized in that in described step b, concentrating under reduced pressure condition is 50-60 ℃, vacuum tightness < 0.1MPa.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829737A (en) * | 2015-04-30 | 2015-08-12 | 华南理工大学 | Crude raspberry leaf polysaccharide, and preparation method and application thereof |
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| CN103191223A (en) * | 2013-04-16 | 2013-07-10 | 吉林化工学院 | Process for extracting total flavonoids in hawthorns by adopting composite enzymatic hydrolysis method to aid ultrasonic action |
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Patent Citations (4)
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| CN1068479A (en) * | 1991-07-12 | 1993-02-03 | 北京市食品研究所 | The separating of hawthorn pectin and fruit juice, purification, method for concentration |
| WO2003047533A2 (en) * | 2001-11-29 | 2003-06-12 | Umwelttechnik Georg Fritzmeier Gmbh & Co. | Composition for treating the surface of the skin |
| CN102755405A (en) * | 2012-07-02 | 2012-10-31 | 吉林金麦通制药有限公司 | Fructus crataegi leaf water extract, preparation containing same and preparation method pf fructus crataegi leaf water extract |
| CN103191223A (en) * | 2013-04-16 | 2013-07-10 | 吉林化工学院 | Process for extracting total flavonoids in hawthorns by adopting composite enzymatic hydrolysis method to aid ultrasonic action |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104829737A (en) * | 2015-04-30 | 2015-08-12 | 华南理工大学 | Crude raspberry leaf polysaccharide, and preparation method and application thereof |
| CN104829737B (en) * | 2015-04-30 | 2017-09-29 | 华南理工大学 | A kind of palmleaf raspberry leaf Thick many candies and preparation method and application |
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Application publication date: 20140319 |