CN101766682A - Process for extracting and purifying total alkaloids of Sophora alopecuroides - Google Patents
Process for extracting and purifying total alkaloids of Sophora alopecuroides Download PDFInfo
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- CN101766682A CN101766682A CN200810246673A CN200810246673A CN101766682A CN 101766682 A CN101766682 A CN 101766682A CN 200810246673 A CN200810246673 A CN 200810246673A CN 200810246673 A CN200810246673 A CN 200810246673A CN 101766682 A CN101766682 A CN 101766682A
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Abstract
The invention discloses a novel process for extracting and purifying alkaloids of Sophora alopecuroides, which is simple, feasible, reasonable and suitable for industrial production. The process comprises the following steps: taking Sophora alopecuroides seeds as raw materials, extracting the total alkaloids of the Sophora alopecuroides by the ethanol impregnation and ultrasonic method, extracting the total alkaloids with an organic solvent, and refining the total alkaloids by the silica gel chromatography. When the active ingredients are purified by utilizing the method, transfer rate of the active ingredients is high and the loss of the effective ingredients is less, thereby achieving the purposes of reducing the production cost and improving the economic benefit.
Description
Technical field
The present invention relates to field of pharmaceutical preparations, disclose matrine and two kinds of monomeric extraction separation of Flos Sophorae alkali in a kind of extraction and purification process of Herba Sophorae alopecuroidis total alkaloids, particularly total alkali.
Background technology
Herba Sophorae alopecuroidis belongs to cassia leguminous plant, is distributed widely in the NORTHWEST CHINA area.Its effective ingredient-alkaloid has important pharmacologically active and application prospect at antitumor, antibiotic, anti-arrhythmia, anti-hepatitis B, aspect such as exempt from service.The pharmacological action of Sophora alopecuroides alkali mainly contains:
(1) matrine in the antitumor action alkaloid can obviously suppress human erythroleukemia cell's strain K562 cell and enters the S phase, suppresses its dna replication dna, suppresses its multiplication capacity; It has inhibitory action to the growing multiplication of human liver cell HepG2, the growth performance of HepG2 is weakened or disappears; Sophocarpine is 31%-56% to the suppression ratio of S180, S27, L1210, and W256 is also had certain life prolongation effect.Sophoridine is 30%-60% to the 10 system rates that press down of mice-transplanted tumors such as Lewis lung cancer.Oxymatrine can induce human breast cancer cell MCF-7 that apoptosis takes place, and oxymatrine and cyclophosphamide share, and the ehrlich carcinoma solid type is had coordinate repression.
(2) antibiotic, antiviral, antiinflammatory, immunization total alkaloid of sophora alopecuroide are external all has bacteriostasis to kind 206 strain experimental bacteria surplus 10, and bacteriostasis is stronger under alkaline environment.Sophoridine, matrine, oxymatrine have antibacterial activity in various degree.Herba Sophorae alopecuroidis total alkali and six kinds of monosomic alkali (matrine, oxymatrine, aloperine, sophoridine, Oxysophoridine sophocarpine) have tangible anti-Ke Saji B papova CVB3 effect.Oxymatrine has direct anti-hepatitis B virus effect, and the HbeAg negative conversion rate is 42.8%, and the HBV-DNA negative conversion rate is 41.8%.Matrine, oxymatrine, sophocarpine and aloperine all have the significantly antiinflammatory action similar to hydrocortisone to the various acute exudative inflammation.Seven kinds of alkaloids can both suppress antibody forming cell's generation, suppress the generation of antibody, and the vigor of serum lysozyme except that the oxidation matrine, is all had inhibitory action.Herba Sophorae alopecuroidis total alkali has and improves the exempt from service effect of function of cell.
(3) the multiple alkaloid of effect Herba Sophorae alopecuroidis class to cardiovascular system has remarkable and sure effect aspect heart tonifying and the anti-arrhythmia.Aloperine, sophocarpine, sophoridine, matrine, sophoramine, oxymatrine all can resist the experimental arrhythmia that kank bundle etc. brings out of coming of age by aconitine, ouabain, chloroform-epinephrine, BaCl2, and mostly are the chamber arrhythmia.Sophoridine can alleviate the degree of necrosis of ischemic myocardium, also can improve the ischemic myocardium energy metabolism, significantly dwindles myocardial infarct size.
(4) effect Oxysophoridine and the oxymatrine to the central nervous system all has central inhibitory action, shows as tranquilizing soporific.Matrine, sophocarpine react bitterly to chemical stimulation and thermostimulation induced mice all obvious inhibitory action, also can reduce the body temperature of normal mouse.
(5) anti-liver injury effect matrine is by denying the IL-1 of emiocytosis to macrophage, liver branch, IL-6, and the inhibition of TNF-α and TNB-β has the effect of anti-hepatic fibrosis, also has the effect of the anti-liver damage of exempting from service.The apoptosis of oxymatrine barbital sodium capable of blocking and the inductive mouse liver cell of endotoxin (LPS), oxymatrine also can suppress hepatic fibrosis.
(6) antiallergic and antiasthmatic effect oxymatrine can suppress IgE and discharge histamine by the mastocyte that antigen causes, membrane fluidity is reduced, but do not change the cAMP level of P81 cell, and having disclosed oxymatrine has anti-allergic effects.Therefore sophocarpine, matrine can we can say that they have antiasthmatic effect obviously to the effect of antihistaminic, the excited tracheal smooth muscle of acetylcholine.
Biology total alkali commonly used extracting method be solvent extraction method, comprise infusion process, percolation, decocting method, circumfluence method, continuous backflow method.Because these method technologies are loaded down with trivial details, extraction time is long, influences the productive rate of effective ingredient.The alkaloid kind is many in the Herba Sophorae alopecuroidis in addition, and structure and character are approaching, has brought certain difficulty to separation and purification.Present stage systematically extracts, the practical art of separation, purification Sophora alopecuroides alkali is also very immature, the particularly production of alkaloid monomer, its production cost height, complex process.
Summary of the invention:
The purpose of this invention is to provide Sophora alopecuroides alkaline extraction, the new technology for purifying of a kind of simple possible, reasonable, suitable suitability for industrialized production, reach the purpose that reduces production costs and increase economic efficiency.When adopting this method that active component is purified, active component rate of transform height, loss of effective components is few.
The present invention is achieved through the following technical solutions.
With the sophora alopecuroide is raw material, adopts alcohol dipping to add ultrasonic method and extracts Herba Sophorae alopecuroidis total alkaloids, utilizes organic solvent that total alkali is extracted, by the refining total alkali of silica gel chromatography.
Wherein, extracting solvent when extracting biology total alkali is ethanol, and extracting liquid pH value is between 0.3-1.1, and optimal pH is 0.5; Reflux extracting time is between 1h-3h, and Best Times is 3h; The supersound process time is advisable at 5min-20min; Supersonic frequency is 20kH-30kHz, and optimum frequency is 28kHz.
Wherein, when extracting, extractant comprises petroleum ether, ether, chloroform, ethyl acetate, acetone, n-butyl alcohol, and preferred solvent is a chloroform.During the alkaloid extraction, pH value of solution is between 10-11, and best pH is 10.5.It is 6 times that extraction times is preferably.
Wherein, during the refined biological total alkali, select for use 100 order silica gel to carry out chromatography, separation eluent is chloroform and methanol.Adopt the ratio that constantly in chloroform, increases methanol to carry out eluting.Collect eluent, detect, when detecting inanimate object alkali, stop with the TLC method.Merge each eluting solvent liquid, concentrate drying promptly gets biology total alkali.
The specific embodiment
Further specify the present invention below in conjunction with the specific embodiment.It should be noted that embodiment only to be used to the present invention is described and do not limit the present invention in any way.
Embodiment 1: the Herba Sophorae alopecuroidis total alkaloids extraction process
Accurately take by weighing the 1Kg sophora alopecuroide, be divided into 10 parts after the pulverizing, use 55%-85% ethanol, the pH that extracts solvent is respectively 0.3-1.1, and return time is respectively 1-5h, the supersound process time is 5-30s respectively, supersonic frequency is respectively 28kHz, 45kHz lixiviate, and lixiviating solution filters and with the filtrate evaporate to dryness, residue is made 5.00ml solution with dehydrated alcohol, use the bromothymol blue colorimetric method for determining, calculate matrine content and matrine extraction ratio.
Accurately take by weighing 10 parts of sophora alopecuroide powder, every part of 1.00g, with ethanol is digestion agent, with above-mentioned experiment of single factor gained result is foundation, determine that the level and the span of these four factors of pH of ultrasound intensity, digestion agent concentration and ultrasonic time, solution carry out orthogonal design, draw the optimum extraction process condition and be: concentration of alcohol 65%; The hydrochloric acid of extractant pH0.5; Supersound extraction frequency 28kHz; Extraction time 20min, the alkaloid extraction rate is 75.76%.
Contain oxymatrine and sophoridine in the Herba Sophorae alopecuroidis total alkaloids.
Embodiment 2: the Herba Sophorae alopecuroidis total alkaloids extraction process
PH is 10-11, has selected solvent petroleum ether, ether, chloroform, ethyl acetate, acetone, the n-butyl alcohol of 6 kinds of opposed polarities that the alkaloids extract after decolouring is carried out telling extraction phase through 3-8 extraction experiments, the thin layer chromatography inspection.Determine extraction process.Optimised process is: pH is 10.5, is solvent with the chloroform, and through 6 extractions, alkaloidal extraction yield has reached and tended towards stability.
Embodiment 3: the Herba Sophorae alopecuroidis total alkaloids purifying process
The Radix Sophorae Flavescentis total alkaloids post separates elution requirement and carries out eluting for adopting the ratio that constantly increases methanol in chloroform.V (chloroform): V (methanol)=linear gradient elution method was carried out eluting to silicagel column in 9: 1 in employing; Reuse V (chloroform): V (methanol)=8.5: 1.5 eluting; After use V (chloroform): V (methanol)=8: 2 eluting instead.Use the acetone crystallize, testing result is respectively matrine, oxymatrine.And all reached 98% purity.
Claims (9)
1. the extraction and purification process of a Herba Sophorae alopecuroidis total alkaloids is characterized in that, is raw material with the sophora alopecuroide, adopts alcohol dipping to add ultrasonic method and extracts Herba Sophorae alopecuroidis total alkaloids, utilizes organic solvent that total alkali is extracted, by the refining total alkali of silica gel chromatography.
2. extraction process as claimed in claim 1 is characterized in that, extracting solvent when extracting biology total alkali is ethanol, and extracting liquid pH value is between 0.3-1.1, and optimal pH is 0.5; Reflux extracting time is between 1h-3h, and Best Times is 3h; The supersound process time is advisable at 5min-20min; Supersonic frequency is 20kH-30kHz, and optimum frequency is 28kHz.
3. extraction process as claimed in claim 1 is characterized in that, when extracting, extractant comprises petroleum ether, ether, chloroform, ethyl acetate, acetone, n-butyl alcohol, and preferred solvent is a chloroform.
4. extraction process as claimed in claim 1 is characterized in that, during the alkaloid extraction, pH value of solution is between 10-11, and best pH is 10.5.
5. extraction process as claimed in claim 1 is characterized in that, extraction times is preferably 6 times.
6. purifying process as claimed in claim 1 is characterized in that, selects for use 100 order silica gel to carry out chromatography.
7. purifying process as claimed in claim 1 is characterized in that, separation eluent is chloroform and methanol.
8. purifying process as claimed in claim 7 is characterized in that, adopts the ratio that constantly increases methanol in chloroform to carry out eluting.
9. purifying process as claimed in claim 7 is characterized in that, collects eluent, detects with the TLC method, stops when detecting inanimate object alkali.Merge each eluting solvent liquid, concentrate drying promptly gets biology total alkali.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102585022A (en) * | 2011-01-14 | 2012-07-18 | 天津市医药科学研究所 | Method for extracting polysaccharides from decoction dregs left after extraction of total alkaloids of sophora alopecuroides |
| CN102875552A (en) * | 2012-10-12 | 2013-01-16 | 塔里木大学 | Composite solvent for efficiently extracting alkaloids |
| CN105030889A (en) * | 2015-09-08 | 2015-11-11 | 保定冀中药业有限公司 | Sophora alopecuroides oral liquid and preparing method thereof |
| CN105663226A (en) * | 2016-04-21 | 2016-06-15 | 新疆维吾尔自治区维吾尔医药研究所 | Application of TASa (Total Alkaloids of Sophora alopecuroides) to preparation of anti-anxiety medicine |
| CN107998175A (en) * | 2017-12-29 | 2018-05-08 | 常州市阿曼特化工有限公司 | A kind of preparation method for the itching-relieving cream for treating seborrhea |
-
2008
- 2008-12-29 CN CN200810246673A patent/CN101766682A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102585022A (en) * | 2011-01-14 | 2012-07-18 | 天津市医药科学研究所 | Method for extracting polysaccharides from decoction dregs left after extraction of total alkaloids of sophora alopecuroides |
| CN102585022B (en) * | 2011-01-14 | 2014-06-11 | 天津市医药科学研究所 | Method for extracting polysaccharides from decoction dregs left after extraction of total alkaloids of sophora alopecuroides |
| CN102875552A (en) * | 2012-10-12 | 2013-01-16 | 塔里木大学 | Composite solvent for efficiently extracting alkaloids |
| CN105030889A (en) * | 2015-09-08 | 2015-11-11 | 保定冀中药业有限公司 | Sophora alopecuroides oral liquid and preparing method thereof |
| CN105030889B (en) * | 2015-09-08 | 2019-05-21 | 保定冀中药业有限公司 | A kind of Sophora alopecuroide oral solution and preparation method thereof |
| CN105663226A (en) * | 2016-04-21 | 2016-06-15 | 新疆维吾尔自治区维吾尔医药研究所 | Application of TASa (Total Alkaloids of Sophora alopecuroides) to preparation of anti-anxiety medicine |
| CN107998175A (en) * | 2017-12-29 | 2018-05-08 | 常州市阿曼特化工有限公司 | A kind of preparation method for the itching-relieving cream for treating seborrhea |
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Application publication date: 20100707 |