CN105273094A - Method for rapid separation of Ligusticum chuanqiong polysaccharide - Google Patents
Method for rapid separation of Ligusticum chuanqiong polysaccharide Download PDFInfo
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- CN105273094A CN105273094A CN201510216957.4A CN201510216957A CN105273094A CN 105273094 A CN105273094 A CN 105273094A CN 201510216957 A CN201510216957 A CN 201510216957A CN 105273094 A CN105273094 A CN 105273094A
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Abstract
The invention relates to a method for rapid separation of Ligusticum chuanqiong polysaccharide, and refers in particular to extraction of Ligusticum chuanqiong polysaccharide through a microwave-assisted double-water-phase system. Ligusticum chuanqiong root tubers are subjected to drying, crushing and degreasing, mixing with an ethanol-inorganic salt double-water-phase extracting solution is carried out, microwave extraction, centrifugation and separation of the alcohol phase are carried out, the alcohol phase is subjected to ethanol precipitation and drying, and Ligusticum chuanqiong polysaccharide is obtained. In the method, extraction of Ligusticum chuanqiong polysaccharide is carried out through microwave-assisted double-water-phase, polysaccharide is dissolved in an organic solvent fully in a short time, extraction time is saved greatly, proteins and color can be removed while Ligusticum chuanqiong polysaccharide is extracted, the polysaccharide recovery rate is more than 80%, the protein removal rate is more than 90%, and the prepared Ligusticum chuanqiong polysaccharide has high activity at the aspect of removing hydroxyl radicals.
Description
Technical field
The present invention relates to separation of biopolymer and extract field, particularly relate to a kind of method of Ligusticum wallichii polysaccharide sharp separation.
Background technology
Ligusticum wallichii is samphire Ligusticum wallichii
ligusticumchuanxiongthe dry rhizome of Hort, has effect of blood-activating and qi-promoting, wind-expelling pain-stopping.Ligusticum wallichii is the traditional Chinese medicine of China, is also famous Genuine crude drugs in Sichuan, according to statistics, and domestic annual output Ligusticum wallichii 5 × 10
6~ 6 × 10
6kg, in the 564 kinds of prescribed preparations recorded in version " Chinese Pharmacopoeia " I portion in 2005 and single preparation, what use Ligusticum wallichii has 85 kinds, and account for that pharmacopeia records Chinese patent medicine 15%.Ligusticum wallichii contains the multiple compounds such as multiple lactone, alkaloids, phenols and volatile oil, and research in recent years finds that Ligusticum wallichii polysaccharide has the function of anticancer growth.Therefore to the research of Ligusticum wallichii polysaccharide function and application thereof, there are bright prospects, the separation and Extraction of current Ligusticum wallichii polysaccharide has alkaline process, ultrasonic assistant method, microwave assisting method and enzyme process, Ligusticum wallichii separation of polysaccharides also will carry out the process of decolouring deproteinated, the loaded down with trivial details much time reagent of program after extracting.Research about double-aqueous phase system extraction Ligusticum wallichii polysaccharide has no report, and the patent that Ligusticum wallichii separation of polysaccharides is extracted also has no open.
Summary of the invention
The technical problem that the present invention solves is a kind of method providing Ligusticum wallichii polysaccharide sharp separation, and the Ligusticum wallichii polysaccharide extract rate extracted in the short period of time is high, and protein removal rate is also high simultaneously, reaches the object of rapid extraction purification of target product.
The method of a kind of Ligusticum wallichii polysaccharide sharp separation provided by the invention, comprises the steps:
(1) double-aqueous phase system is formed: secure ph scope is the system damping fluid of 3.0-8.0, by ethanol and inorganic salt system buffer solution, mixing, form the double-aqueous phase system of extraction Ligusticum wallichii polysaccharide, the ultimate density scope of inorganic salt in system is 10%-40%, the ethanol ultimate density scope in system is 20%-50%;
(2) Ligusticum wallichii dried root is pulverized, and sieves, obtains 20 order-80 order Szechwan Lovage Rhizomes;
(3) powder is joined double-aqueous phase system according to the ratio that solid-to-liquid ratio is 1:10 to 1:60 and make extraction solution;
(4) by extraction solution at 100W-600W, microwave treatment 5min-30min at 30 DEG C-50 DEG C;
(5) by extraction liquid 2000-5000 turn/min under centrifugal 5-15min;
(6) add ethanol to centrifuged supernatant, make the final ethanol concentration in solution be 35%-85%, mixing, 4 DEG C of hold over night;
(7) by ethanol 2000-5000 turn/min under centrifugal 5-15min, collecting precipitation;
(8) drying will be precipitated, make Ligusticum wallichii polysaccharide powder.
Preferably, in step (1), double-aqueous phase system pH of cushioning fluid scope is 5.5-6.5, and the ultimate density scope of inorganic salt in system is 20%-30%, and the ultimate density scope of ethanol in system is 25%-35%.
Preferably, in step (2), Ligusticum wallichii block root is dried to constant weight at 55 DEG C of-65 DEG C of temperature, is pulverized by high-speed tissue mashing machine and obtain Szechwan Lovage Rhizome, powder is crossed 30-50 mesh sieve, make Szechwan Lovage Rhizome.
Preferably, in step (3), powder is joined double-aqueous phase system according to the ratio that solid-to-liquid ratio is 1:35-1:45 and make extraction solution.
Preferably, in step (4), by extraction solution at 300W-500W, microwave treatment 10min-20min at 30 DEG C-50 DEG C.
Preferably, in step (5), by extraction liquid 3500-4500 turn/min under centrifugal 5-15min.
Preferably, in step (6), the ethanol final concentration scope in centrifuged supernatant is at 60%-70%.
Preferably, in step (7) a metallic, ethanol 3500-4500 turn/min under centrifugal 5-15min.
Preferably, in step (8), be deposited in negative 20 DEG C of lyophilizes.
Compared with prior art, the method for double-aqueous phase system provided by the invention extraction Ligusticum wallichii polysaccharide, can while Ligusticum wallichii polysaccharide is extracted into phase by impurity extraction such as protein to lower phase or at two-phase interface, thus raising target product purity; In conjunction with microwave-assisted extraction technique, greatly can improve the percentage extraction of Ligusticum wallichii polysaccharide, shorten extraction time, save cost.
Embodiment
In order to those skilled in the art can understand technical scheme provided by the present invention better, set forth below in conjunction with specific embodiment.
The method of a kind of Ligusticum wallichii polysaccharide sharp separation of the present invention, comprises the steps:
(1) Ligusticum wallichii block root is dried to constant weight at 60 DEG C, is pulverized by high-speed tissue mashing machine and obtain Szechwan Lovage Rhizome, powder is crossed 40 mesh sieves, obtain Szechwan Lovage Rhizome;
(2) powder is added double-aqueous phase system according to the ratio that solid-to-liquid ratio is 1:40 and make extraction solution, double-aqueous phase system consists of the ethanol of 32%, the ammonium sulfate of 24%, and system pH is 6.0;
(3) extraction solution is placed in microwave extracting apparatus, at 400w, at 40 DEG C, extracts 15min;
(4) extraction liquid after radiation being terminated is centrifugal 10min under 4000 turns/min;
(5) add ethanol to centrifuged supernatant, make the final ethanol concentration in solution be 65%, mixing, 4 DEG C of hold over night;
(6) by ethanol centrifugal 10min under 4000 turns/min, collecting precipitation;
(7) negative 20 DEG C of lyophilizes will be deposited in, make Ligusticum wallichii polysaccharide powder; Ligusticum wallichii polysaccharide recovery is more than 80%, and purity reaches more than 90%, and scavenging hydroxyl activity is high.
To the above-mentioned explanation of the disclosed embodiments, professional and technical personnel in the field are realized or uses the present invention.To be apparent for those skilled in the art to the multiple amendment of these embodiments, General Principle as defined herein can without departing from the spirit or scope of the present invention, realize in other embodiments.Therefore, the present invention can not be restricted to these embodiments shown in this article, but will meet the widest scope consistent with principle disclosed herein and features of novelty.
Claims (9)
1. a method for Ligusticum wallichii polysaccharide sharp separation, is characterized in that, comprises the steps:
(1) secure ph scope is the system damping fluid of 5.0-7.0, by ethanol and inorganic salt system buffer solution, mixing, forms the double-aqueous phase system of extraction Ligusticum wallichii polysaccharide, the ultimate density scope of inorganic salt in system is 10%-40%, and the ultimate density scope of ethanol in system is 20%-50%;
(2) Ligusticum wallichii dried root is pulverized, and sieves, obtains 20 order-80 order Szechwan Lovage Rhizomes;
(3) powder is joined double-aqueous phase system according to the ratio that solid-to-liquid ratio is 1:10 to 1:60 and make extraction solution;
(4) by extraction solution at 100W-600W, microwave treatment 5min-30min at 30 DEG C-50 DEG C;
(5) by extraction liquid 2000-5000 turn/min under centrifugal 5min-15min;
(6) add ethanol to centrifuged supernatant, make the final ethanol concentration in solution be 35%-85%, mixing, 4 DEG C of hold over night;
(7) by ethanol 2000-5000 turn/min under centrifugal 5min-15min, collecting precipitation;
(8) drying will be precipitated, make Ligusticum wallichii polysaccharide powder.
2. the method for Ligusticum wallichii polysaccharide sharp separation according to claim 1, it is characterized in that, in step (1), by the system buffer solution of ethanol and inorganic salt pH5.5-pH6.5, mixing, form the double-aqueous phase system of extraction Ligusticum wallichii polysaccharide, the ultimate density scope of inorganic salt in system is 20%-30%, the ethanol ultimate density scope in system is 25%-35%.
3. the method for Ligusticum wallichii polysaccharide sharp separation according to claim 1, it is characterized in that, in step (2), Ligusticum wallichii block root is dried to constant weight at 55 DEG C of-65 DEG C of temperature, pulverized by high-speed tissue mashing machine and obtain Szechwan Lovage Rhizome, powder is crossed 30 mesh sieve-50 mesh sieves and obtain powder.
4. the method for Ligusticum wallichii polysaccharide sharp separation according to claim 1, is characterized in that, in step (3), Szechwan Lovage Rhizome joins double-aqueous phase system according to the ratio that solid-to-liquid ratio is 1:35 to 1:45 and makes extraction solution.
5. the method for Ligusticum wallichii polysaccharide sharp separation according to claim 1, is characterized in that, in step (4), by extraction solution at 300w-500w, and microwave treatment 10min-20min at 30 DEG C-50 DEG C.
6. the method for Ligusticum wallichii polysaccharide sharp separation according to claim 1, is characterized in that, in step (5), extraction liquid 3000 turns/min-4000 turn/min under centrifugal 5min-15min.
7. the method for Ligusticum wallichii polysaccharide sharp separation according to claim 1, is characterized in that, in step (6), the ethanol final concentration in centrifuged supernatant is 60%-70%, in low temperature 4 DEG C of hold over night.
8. the method for Ligusticum wallichii polysaccharide sharp separation according to claim 1, is characterized in that, in step (7) a metallic, extraction liquid 3000 turns/min-4000 turn/min under centrifugal 5min-15min.
9. the method for Ligusticum wallichii polysaccharide sharp separation according to claim 1, is characterized in that, in step (8), ethanol pellet is in negative 20 DEG C of lyophilizes.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105943473A (en) * | 2016-07-06 | 2016-09-21 | 邵阳学院 | Mixed extracting liquid for rhizoma polygonati odorati polysaccharide and oyster mushroompolysaccharide and application thereof |
| CN108329397A (en) * | 2018-03-08 | 2018-07-27 | 西北农林科技大学 | A method of addition inorganic salts improve Hubei Sorbus alnifloria leaf polyose alcohol precipitation efficiency |
| CN109943893A (en) * | 2019-02-27 | 2019-06-28 | 唐卫兵 | A kind of preparation method of the warming natural nano bamboo fibre/cotton fiber composite material of long acting antibiotic |
| CN110655587A (en) * | 2019-09-24 | 2020-01-07 | 澜海(福建)生物科技有限公司 | Preparation method of bletilla striata polysaccharide |
| CN111777693A (en) * | 2020-08-17 | 2020-10-16 | 重庆医科大学附属第二医院 | Ligusticum wallichii homogeneous polysaccharide and extraction method and application thereof |
| CN112029008A (en) * | 2020-09-16 | 2020-12-04 | 天津中新药业集团股份有限公司中新制药厂 | Ligusticum wallichii crude polysaccharide with special molecular weight, extraction process from dregs of a decoction and application |
| CN112029007A (en) * | 2020-09-16 | 2020-12-04 | 天津中新药业集团股份有限公司中新制药厂 | Defatted deproteinized macromolecular ligusticum wallichii polysaccharide and preparation method of rhizoma ligustici wallichii polysaccharide from dregs |
| CN113512129A (en) * | 2021-08-23 | 2021-10-19 | 石河子大学 | Method for extracting polysaccharide from plant |
| CN115403677A (en) * | 2021-05-28 | 2022-11-29 | 纳米及先进材料研发院有限公司 | Method for extracting polysaccharide |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105943473A (en) * | 2016-07-06 | 2016-09-21 | 邵阳学院 | Mixed extracting liquid for rhizoma polygonati odorati polysaccharide and oyster mushroompolysaccharide and application thereof |
| CN105943473B (en) * | 2016-07-06 | 2018-06-22 | 邵阳学院 | A kind of fragrant solomonseal rhizome polyoses and mushroom polysaccharide hybrid extraction liquid and its application |
| CN108329397A (en) * | 2018-03-08 | 2018-07-27 | 西北农林科技大学 | A method of addition inorganic salts improve Hubei Sorbus alnifloria leaf polyose alcohol precipitation efficiency |
| CN108329397B (en) * | 2018-03-08 | 2020-08-14 | 西北农林科技大学 | Method for improving alcohol precipitation efficiency of sorbus hupehensis leaf polysaccharide by adding inorganic salt |
| CN109943893A (en) * | 2019-02-27 | 2019-06-28 | 唐卫兵 | A kind of preparation method of the warming natural nano bamboo fibre/cotton fiber composite material of long acting antibiotic |
| CN110655587A (en) * | 2019-09-24 | 2020-01-07 | 澜海(福建)生物科技有限公司 | Preparation method of bletilla striata polysaccharide |
| CN111777693A (en) * | 2020-08-17 | 2020-10-16 | 重庆医科大学附属第二医院 | Ligusticum wallichii homogeneous polysaccharide and extraction method and application thereof |
| CN112029008A (en) * | 2020-09-16 | 2020-12-04 | 天津中新药业集团股份有限公司中新制药厂 | Ligusticum wallichii crude polysaccharide with special molecular weight, extraction process from dregs of a decoction and application |
| CN112029007A (en) * | 2020-09-16 | 2020-12-04 | 天津中新药业集团股份有限公司中新制药厂 | Defatted deproteinized macromolecular ligusticum wallichii polysaccharide and preparation method of rhizoma ligustici wallichii polysaccharide from dregs |
| CN115403677A (en) * | 2021-05-28 | 2022-11-29 | 纳米及先进材料研发院有限公司 | Method for extracting polysaccharide |
| CN113512129A (en) * | 2021-08-23 | 2021-10-19 | 石河子大学 | Method for extracting polysaccharide from plant |
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