CN105111327A - Extraction method for rapidly separating allium macrostemon active polysaccharide on basis of ultrafiltration method - Google Patents
Extraction method for rapidly separating allium macrostemon active polysaccharide on basis of ultrafiltration method Download PDFInfo
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Abstract
The invention discloses an extraction method for rapidly separating allium macrostemon active polysaccharide on the basis of an ultrafiltration method. The extraction method comprises the following steps: (1), taking fresh allium macrostemon, washing, drying, smashing, and screening through a 60-mesh sieve so as to obtain smashed allium macrostemon; (2), carrying out reflux degreasing on the smashed allium macrostemon obtained in the step (1) with petroleum ether or ethyl ether; (3), adding water into residues obtained in the step (2) for hot water extraction for multiple times and mixing so as to obtain an extraction solution; (4), centrifuging the extraction solution obtained in the step (3) so as to obtain supernatant; (5), carrying out ultrafiltration on the supernatant obtained in the step (4) by adopting ultrafiltration equipment so as to obtain permeate liquid and trapped fluid; (6), adding ethyl alcohol into trapped fluid obtained in the step (5) until the final concentration is 70%, placing at room temperature and centrifuging so as to obtain solid precipitates; (7), washing the solid precipitates obtained in the step (6) with absolute ethyl alcohol, acetone and ethyl ether sequentially, performing vacuum drying, so as to obtain the allium macrostemon active polysaccharide. The allium macrostemon active polysaccharide prepared by adopting the technical scheme is grey white flocculent powder and the uronic acid content of the allium macrostemon active polysaccharide is 24.73%.
Description
Technical field
The present invention relates to a kind of extracting method of vegetable polysaccharides, particularly relate to a kind of extracting method based on active polysaccharide in hyperfiltration process sharp separation Longstamen Onion Bulb newly.
Background technology
Longstamen Onion Bulb (
alliummacrostemonbunge) one of 87 kinds of medicine food dual purpose plants announced for the Ministry of Health 2002, another name Chinese wild onion, Allium macrostemon, mountain garlic, bitter garlic, little garlic, little root vegetables, wild green onion, Longstamen Onion Bulb are first-class, for Liliaceae allium per nnial herb, be distributed widely in the plains region of the states such as China, Japan and Korea S, eat more, its dry bulb also can be used as medicine, and medicinal Longstamen Onion Bulb is plant Allium macrostemon
a.macrostemonor Chinese onion Bge.
a.chinensisG.Dondry bulb.Longstamen Onion Bulb taste is pungent, bitter, warm in nature, nontoxic, have regulate the flow of vital energy, wide chest, activate yang, effect of dissipating bind, the traditional Chinese medical science is used for the treatment of shouting pain uncomfortable in chest for a long time, rush down dysentery after heavy, lung qi breathe heavily the diseases such as anxious.Certain relation is had with the treatment of the cardiovascular disordeies such as the stenocardia in modern medicine, atherosclerosis, myocardial infarction.As natural bioactive ingredients, research has found that polysaccharide has the several functions such as anti-oxidant, antitumor, anti-inflammatory and immunomodulatory, and has comparatively significantly corresponding relation between the height of glucuronic acid content and the power of its activity in polysaccharide.
In recent years, from aspects such as the structure activity relationships of optimal extraction technology, sterling preparation, structural analysis qualification, screening active ingredients evaluation and structure and function, the research that comparatively system is deep is carried out to Longstamen Onion Bulb polysaccharide, find that a kind of glucuronic acid content is higher, there is the acidic polysaccharose compared with strong biological activity.But up to now, the extracting method of Longstamen Onion Bulb polysaccharide is only limitted to the traditional way of concentrating under reduced pressure, consumes energy high, polysaccharide extraction rate is lower simultaneously.
In " Agriculture of Anhui science ", 2006, in 34 (17), by Xiaxin's Kui, Yang Haixia, Li Chun, in " Extraction Technology of Polysaccharide from Allium macrosttemon B research " article that Yin Jian delivers, disclose a kind of extracting method of Longstamen Onion Bulb polysaccharide, the scheme of concrete employing is: the Longstamen Onion Bulb dry product powder 200g taking pulverizing, methanol eddy sloughs surface fat, suction filtration, the dregs of a decoction are air-dry, again with 80% alcohol reflux removing small molecular sugar, glycoside, alkaloid etc., the dregs of a decoction are air-dry, then get it filled slag 5g respectively, using water as solvent, adopt different Extracting temperature, different solid-liquid ratios, different extraction times carries out Polyose extraction experiment to the dregs of a decoction, the centrifugal removing impurity of Aqueous extracts, be evaporated to small volume, adding dehydrated alcohol to concentration is 75% precipitation, filter after leaving standstill 24h, with 95% ethanol, dehydrated alcohol, washing with acetone several, vacuum-drying, obtains Longstamen Onion Bulb Crude polysaccharides.Also indicate extracting factor further in literary composition, comprise Extracting temperature, liquid ratio, extraction time, extraction time etc.
But, still there is many deficiencies in this extracting method, extraction yield is lower, in leaching process, rate of loss is higher, under optimal extract process, the average recoveries of Longstamen Onion Bulb polysaccharide is 13.93%, the Longstamen Onion Bulb polysaccharide extracted mostly is the neutral polysaccharide of molecular weight, and the acidic polysaccharose of larger molecular weight accounts for smaller, and thus biological activity is lower.
Summary of the invention
The object of the invention aims to provide a kind of extracting method based on hyperfiltration process sharp separation macrostem onion active polysaccharide of efficient, environmental protection.
For solving the problems of the technologies described above, the technical solution used in the present invention is: based on the extracting method of hyperfiltration process sharp separation macrostem onion active polysaccharide, should comprise the following steps:
(1) get fresh Longstamen Onion Bulb, after clean dry, pulverized 60 mesh sieves, and obtained macrostem onion powder and mince;
(2) minced by the obtained macrostem onion powder in step (1), adopt sherwood oil or aether backflow degreasing, centrifugal segregation supernatant liquor, residue obtained 50 DEG C of oven dry, the liquid ratio that sherwood oil or ether and macrostem onion powder mince is 5:1;
(3) by residue obtained for step (2), add water and carry out hot water extraction, ratio of water to material is 4-25mL/g, Extracting temperature 60-100 DEG C, extraction time 0.5-3h, extracts several times, merges to obtain extracting solution;
(4) by step (3) gained extracting solution, centrifugal, obtain supernatant liquor;
(5) by the supernatant liquor of step (4) gained, adopt ultrafiltration apparatus, application specification 50kD ultra-filtration membrane is 20 ~ 45 DEG C in temperature, and working pressure is carry out ultrafiltration under 0.10-0.40MPa condition, obtains permeate and trapped fluid;
(6) by step (5) gained trapped fluid, add ethanol to final concentration 70%, room temperature is centrifugal after placing, and obtains solid sediment;
(7) by step (6) gained solid sediment, use dehydrated alcohol, acetone, washed with diethylether successively, vacuum-drying, obtain macrostem onion active polysaccharide.
Further improvement is, the eccentricity in described step (5) is 5000r/m, and the time is 10min.
Further improvement is, the eccentricity in described step (7) is 5000rpm, and the time is 10min.
Further improvement is, in described step (1), dry employing bake out temperature is 50 DEG C; In described step (2), adopt sherwood oil backflow degreasing 1 time, time 3h, by residue obtained for step (2), uses 80% ethanol, and small molecules is removed in backflow, centrifugal segregation supernatant liquor, residue obtained oven dry, and the liquid ratio of 80% ethanol and residue is 8:1; In described step (3), backflow removes small molecules 1 time, time 3h; In described step (4), extraction time 1-5 time; In described step (7), storage period is 24h; In described step (8), respectively wash 1 time with dehydrated alcohol, acetone, ether successively, vacuum-drying at 50 DEG C.
Further improvement is, in described step (1), fresh Longstamen Onion Bulb removes fibrous root after cleaning, and steams thoroughly or put in boiling water to scald thoroughly, adopts and dries mode drying; In described step (2), adopt aether backflow degreasing 2 times, each time 2h; In described step (3), extraction time 1-5 time; In described step (6), storage period is 24h; In described step (7), respectively wash 1 time with dehydrated alcohol, acetone, ether successively, vacuum-drying at 50 DEG C.
Adopt such scheme of the present invention, sulfuric acid-meta-hydroxydiphenyl method is adopted to carry out glucuronic acid content mensuration, preparing gained macrostem onion active polysaccharide is the cotton-shaped powder of canescence, its glucuronic acid content 24.73%, far above in permeate and other Longstamen Onion Bulb polysaccharide not adopting hyperfiltration process obtained; Gained macrostem onion active polysaccharide infrared analysis test result shows, at 3500-3250cm
-1wide and strong polysaccharide hydroxyl O-H stretching vibration peak has been there is, 2900-2800cm in scope
-1occur the strong stretching vibration peak of the C-H of polysaccharide in scope, these two peaks are the charateristic avsorption band of polysaccharose substance, wherein at 1750cm
-1place, the strong absorption peak of appearance is the asymmetric stretching vibration of C=O of carboxyl, illustrates that this polysaccharide contains carboxylic group, has greater activity.
Accompanying drawing explanation
Fig. 1 is that the Longstamen Onion Bulb polysaccharide adopting the active polysaccharide that is separated to from Longstamen Onion Bulb of the inventive method and additive method to be separated to contrasts the inhibiting rate after tumour cell BGC-823 effect 24h;
Fig. 2 is embodiment 1 Longstamen Onion Bulb extracting solution macrostem onion active polysaccharide infrared spectrum in ultrafiltration gained trapped fluid.
Embodiment
Embodiment 1: get fresh Longstamen Onion Bulb, cleans, and after 50 DEG C of oven dry, pulverizes 60 mesh sieves, and obtains macrostem onion powder and mince; By obtained crushed material, sherwood oil (liquid ratio 5:1) refluxes degreasing 1 time, time 3h, centrifugal segregation supernatant liquor, residue obtained 50 DEG C of oven dry; Residue after drying, removes small molecules 1 time, time 3h, centrifugal segregation supernatant liquor, residue obtained 50 DEG C of oven dry with 80% ethanol (liquid ratio 8:1) backflow; By residue obtained, add water and carry out hot water extraction, ratio of water to material 4-25mL/g, Extracting temperature 60-100 DEG C, extraction time 0.5-3h, extraction time 1-5 time, merge to obtain extracting solution; By gained extracting solution, centrifugal (5000rpm, 10min), obtains supernatant liquor; By gained supernatant liquor, adopt ultrafiltration apparatus, application specification 50kD ultra-filtration membrane, at temperature (20 ~ 45 DEG C), carries out ultrafiltration under working pressure (0.10-0.40MPa) condition, obtains permeate and trapped fluid; By gained trapped fluid, add ethanol to final concentration 70%, after room temperature placement 24h centrifugal (5000rpm, 10min), obtain solid sediment; By gained throw out, respectively wash 1 time with dehydrated alcohol, acetone, ether successively, vacuum-drying at 50 DEG C, obtain macrostem onion active polysaccharide.
Longstamen Onion Bulb extracting solution macrostem onion active polysaccharide infrared spectrum in ultrafiltration gained trapped fluid shows (as shown in Figure 2), at 3500-3250cm
-1wide and strong polysaccharide hydroxyl O-H stretching vibration peak has been there is, 2900-2800cm in scope
-1occur the strong stretching vibration peak of the C-H of polysaccharide in scope, these two peaks are the charateristic avsorption band of polysaccharose substance.Wherein at 1750cm
-1place, the strong absorption peak of appearance is the asymmetric stretching vibration of C=O of carboxyl, illustrates that this polysaccharide contains carboxylic group, has greater activity.
Embodiment 2: get fresh Longstamen Onion Bulb, cleans, removing fibrous root, steams thoroughly or puts in boiling water and scald thoroughly, after drying, pulverized 60 mesh sieves, and obtained macrostem onion powder and mince; By obtained crushed material, ether (liquid ratio 5:1) refluxes degreasing 2 times, each time 2h, centrifugal segregation supernatant liquor, residue obtained 50 DEG C of oven dry; By residue obtained, add water and carry out hot water extraction (ratio of water to material 4-25mL/g), Extracting temperature 60-100 DEG C, extraction time 0.5-3h, extraction time 1-5 time, merges to obtain extracting solution; By gained extracting solution, centrifugal (5000rpm, 10min), obtains supernatant liquor; By gained supernatant liquor, adopt ultrafiltration apparatus, application specification 50kD ultra-filtration membrane, at temperature (20 ~ 45 DEG C), carries out ultrafiltration under working pressure (0.10-0.40MPa) condition, obtains permeate and trapped fluid; By gained trapped fluid, add ethanol to final concentration 60%, after room temperature placement 24h centrifugal (5000rpm, 10min), obtain solid sediment; By gained throw out, respectively wash 1 time with dehydrated alcohol, acetone, ether successively, vacuum-drying at 50 DEG C, obtain macrostem onion active polysaccharide.
In above-mentioned enforcement 1,2, sulfuric acid-meta-hydroxydiphenyl method is adopted to carry out glucuronic acid content mensuration, preparing gained macrostem onion active polysaccharide is the cotton-shaped powder of canescence, its glucuronic acid content 24.73%, with employing " Agriculture of Anhui science ", 2006, in 34 (17), compared by disclosed common extracting method such as Xiaxin's Kuis, in the extract not adopting hyperfiltration process to obtain, acidic polysaccharose is obviously on the low side, and the acidic polysaccharose content that the inventive method obtains is higher.
Embodiment is above described in detail the solution of the present invention, but the invention is not restricted to above-described embodiment, in the ken that art those of ordinary skill possesses, can also make a variety of changes under the prerequisite not departing from present inventive concept.
Claims (5)
1., based on an extracting method for hyperfiltration process sharp separation macrostem onion active polysaccharide, comprise the following steps:
(1) get fresh Longstamen Onion Bulb, after clean dry, pulverized 60 mesh sieves, and obtained macrostem onion powder and mince;
(2) minced by the obtained macrostem onion powder in step (1), adopt sherwood oil or aether backflow degreasing, centrifugal segregation supernatant liquor, residue obtained 50 DEG C of oven dry, the liquid ratio that sherwood oil or ether and macrostem onion powder mince is 5:1;
(3) by residue obtained for step (2), add water and carry out hot water extraction, ratio of water to material is 4-25mL/g, Extracting temperature 60-100 DEG C, extraction time 0.5-3h, extracts several times, merges to obtain extracting solution;
(4) by step (3) gained extracting solution, centrifugal, obtain supernatant liquor;
(5) by the supernatant liquor of step (4) gained, adopt ultrafiltration apparatus, application specification 50kD ultra-filtration membrane is 20 ~ 45 DEG C in temperature, and working pressure is carry out ultrafiltration under 0.10-0.40MPa condition, obtains permeate and trapped fluid;
(6) by step (5) gained trapped fluid, add ethanol to final concentration 70%, room temperature is centrifugal after placing, and obtains solid sediment;
(7) by step (6) gained solid sediment, use dehydrated alcohol, acetone, washed with diethylether successively, vacuum-drying, obtain macrostem onion active polysaccharide.
2. the extracting method based on hyperfiltration process sharp separation macrostem onion active polysaccharide according to claim 1, is characterized in that, the eccentricity in described step (5) is 5000r/m, and the time is 10min.
3. the extracting method based on hyperfiltration process sharp separation macrostem onion active polysaccharide according to claim 1, is characterized in that, the eccentricity in described step (7) is 5000rpm, and the time is 10min.
4. the extracting method based on hyperfiltration process sharp separation macrostem onion active polysaccharide according to any one of claim 1 ~ 3, is characterized in that, in described step (1), dry employing bake out temperature is 50 DEG C; In described step (2), adopt sherwood oil backflow degreasing 1 time, time 3h, by residue obtained for step (2), uses 80% ethanol, and small molecules is removed in backflow, centrifugal segregation supernatant liquor, residue obtained oven dry, and the liquid ratio of 80% ethanol and residue is 8:1; In described step (3), backflow removes small molecules 1 time, time 3h; In described step (4), extraction time 1-5 time; In described step (7), storage period is 24h; In described step (8), respectively wash 1 time with dehydrated alcohol, acetone, ether successively, vacuum-drying at 50 DEG C.
5. the extracting method based on hyperfiltration process sharp separation macrostem onion active polysaccharide according to any one of claim 1 ~ 3, is characterized in that, in described step (1), fresh Longstamen Onion Bulb removes fibrous root after cleaning, and steams thoroughly or put in boiling water to scald thoroughly, adopts and dries mode drying; In described step (2), adopt aether backflow degreasing 2 times, each time 2h; In described step (3), extraction time 1-5 time; In described step (6), storage period is 24h; In described step (7), respectively wash 1 time with dehydrated alcohol, acetone, ether successively, vacuum-drying at 50 DEG C.
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