CN102219786A - Preparation method of sparteine - Google Patents
Preparation method of sparteine Download PDFInfo
- Publication number
- CN102219786A CN102219786A CN2011101515092A CN201110151509A CN102219786A CN 102219786 A CN102219786 A CN 102219786A CN 2011101515092 A CN2011101515092 A CN 2011101515092A CN 201110151509 A CN201110151509 A CN 201110151509A CN 102219786 A CN102219786 A CN 102219786A
- Authority
- CN
- China
- Prior art keywords
- membrane
- tocosamine
- preparation
- concentrated solution
- adds
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Landscapes
- Separation Using Semi-Permeable Membranes (AREA)
Abstract
The invention relates to a preparation method of a sparteine. The method comprises the following steps: a. crushing thermopsis lanceolata seeds, adding 0.5-1% hydrochloric acid or sulfuric acid aqueous solution for cold leaching, adjusting a pH of an extract to neutral, filtering, adding into an ultrafiltration membrane for ultrafiltration, then adding into a nanofiltration membrane for filtering, concentrating through a reverse osmosis membrane to obtain a concentrated solution; b. adjusting a pH of the concentrated solution to 9-10, extracting with dichloromethane, concentrating an extract and separating by a high speed countercurrent chromatography, collecting target components according to an ultraviolet detector spectrum, and drying at a low temperature to finish. Sparteine produced by the method has a high yield, high product content, besides the method can lower energy consumption and reduce pollution.
Description
Technical field:
The present invention relates to a kind of preparation method of Tocosamine, especially a kind ofly adopt the method that membrane sepn and high speed adverse current chromatogram prepare Tocosamine.
Background technology:
Tocosamine, molecular formula C
11H
14ON
2, molecular weight 190.24, molecular structural formula:
Physical properties: tiltedly quadratic prism crystallization (acetone), 152～153 ℃ of fusing points.Soluble in water, ethanol, chloroform, benzene are insoluble to sherwood oil, ether.
Tocosamine different name Cytisine has the effect of cough-relieving apophlegmatic, applies to rescue because of reflectivity breathlessness, shock and the asphyxia neonatorum etc. of performing the operation and various wound causes.Recent research shows, can be used for producing smoking deterent, first aid medicine, antitussive.
Herba Thermopsis Lanceolatae is the seed of the yellow China of dicotyledons pulse family lanceolata, and main component has Tocosamine, thermopsine, homothermopsine, rhombinin, methylcytisine, sparteine; Also containing lupin alkaloid, rhombifoline, thermosamine. leaf contains a small amount of flavonoid compound.Seed contains alkaloid and reaches 5%, and main component is a Tocosamine content about 2%.
Have now and mostly the Tocosamine extraction and purification process is traditional technology, organic reagent extraction, acidizing extraction, alkalization extraction, alumina column or silica gel column chromatography, operations such as acetone crystallization." in the Herba Thermopsis Lanceolatae alkaloid extraction separate and identify " that " Study on Extraction Method of high purity Tocosamine " delivered as Wu Yong etc. and Zhao Baoyu etc. deliver, disclosed method promptly is a traditional technology.Patent (application number 200910023485) " a kind of method of extracting Tocosamine and thermopsine from the yellow magnificent seed of lanceolata ", this invention also is that organic reagent extracts, acidification extraction, alkalization extraction, extracted with diethyl ether, operations such as acetone crystallization.Technological deficiencies such as existing as mentioned above preparation technology exists complicated operation, and yield is low, seriously polluted.
Summary of the invention:
The technological deficiency that the technical problem to be solved in the present invention overcomes existing technology is that a kind of preparation method of Tocosamine is provided.This method is adopted the method that membrane sepn and high speed adverse current chromatogram prepare Tocosamine, can product yield, and reduce and pollute, but industrialization production.
In order to solve the problems of the technologies described above, extractive technique scheme of the present invention is as follows: a kind of preparation method of Tocosamine is characterized in that may further comprise the steps:
A. the Herba Thermopsis Lanceolatae seed is pulverized, and adds 0.5-1% hydrochloric acid or aqueous sulfuric acid cold soaking, and extracting solution is regulated the neutral filtration of pH, adds the ultra-filtration membrane ultrafiltration, adds nanofiltration membrane again and filters, and sees through liquid and concentrates with reverse osmosis membrane, gets concentrated solution;
B. above-mentioned concentrated solution is transferred pH9-10, uses dichloromethane extraction, and extraction liquid concentrates and adopts high speed adverse current chromatogram to separate again, collects target component according to the UV-detector collection of illustrative plates, and cryodrying promptly.
Described ultra-filtration membrane molecular weight cut-off 3000-10000, nanofiltration membrane molecular weight cut-off 300-600.
A kind of in the optional tubular type of described ultra-filtration membrane, nanofiltration membrane and reverse osmosis membrane, rolling and the hollow membrane, a kind of in the optional tynex of material, polyethersulfone, the tetrafluoroethylene.
Described high speed adverse current chromatogram solvent systems is chloroform, ethanol, phosphate sodium dihydrogen buffer solution (pH5-6), blending ratio 3-5: 4-5: 2-3, on be moving phase mutually, is stationary phase mutually down.
Advantage of the present invention is: the process using membrane filtration is a kind of physical separation method of less energy-consumption, and the material quality is had good protection, separated component effectively, and the sample free of losses belongs to the environment-friendly type method; Technology also adopts high speed adverse current chromatogram, and it is to utilize liquid liquid distribution chromatography principle, and the sample separation free of losses has overcome that being difficult to resolve of solid chromatography column analysed, complex operation and produce the defective of a large amount of solid waste.
Further specify the present invention below in conjunction with embodiment, but the scope of protection of present invention is not limited to following embodiment.
Embodiment:
Embodiment 1:
The Herba Thermopsis Lanceolatae seed is pulverized, get 3kg, add 10 times of amount 1% aqueous hydrochloric acid cold soakings 3 times, extracting solution is regulated pH neutrality, filters the hollow tynex ultra-filtration membrane ultrafiltration that the back adds molecular weight cut-off 3000, adds molecular weight cut-off 300 hollow tynex nanofiltration membrane again through liquid and filters, adding hollow tynex reverse osmosis membrane again through liquid concentrates, concentrated solution is transferred pH10, uses dichloromethane extraction 3 times, and extraction liquid is concentrated into small volume.Get chloroform, ethanol, phosphate sodium dihydrogen buffer solution (pH5), mix standing demix at 3: 5: 2 in proportion, take off and be full of the high speed adverse current chromatogram post phase that fixes mutually, start main frame, adjust rotating speed 800rpm, pump into phase, treated that liquid flows out, and adjusts flow velocity 2ml/min, there is sampling valve to advance concentrated solution simultaneously, collect target component according to the UV-detector collection of illustrative plates, preparation continuously, the flow point cryodrying gets Tocosamine 45g, detect content 96.7% through HPLC.
Embodiment 2:
The Herba Thermopsis Lanceolatae seed is pulverized, get 3kg, add 10 times of amount 0.5% aqueous sulfuric acid cold soakings 3 times, extracting solution is regulated pH neutrality, filters the tubular type tetrafluoroethylene ultra-filtration membrane ultrafiltration that the back adds molecular weight cut-off 10000, adds molecular weight cut-off 600 tubular type tetrafluoroethylene nanofiltration membrane again through liquid and filters, adding tubular type tetrafluoroethylene reverse osmosis membrane again through liquid concentrates, concentrated solution is transferred pH9, uses dichloromethane extraction 4 times, and extraction liquid is concentrated into small volume.Get chloroform, ethanol, phosphate sodium dihydrogen buffer solution (pH6), mix standing demix at 5: 5: 3 in proportion, take off and be full of the high speed adverse current chromatogram post phase that fixes mutually, start main frame, adjust rotating speed 900rpm, pump into phase, treated that liquid flows out, and adjusts flow velocity 3ml/min, there is sampling valve to advance concentrated solution simultaneously, collect target component according to the UV-detector collection of illustrative plates, preparation continuously, the flow point cryodrying gets Tocosamine 49g, detect content 97.5% through HPLC.
Embodiment 3:
The Herba Thermopsis Lanceolatae seed is pulverized, get 3kg, add 10 times of amount 0.5% aqueous sulfuric acid cold soakings 3 times, extracting solution is regulated pH neutrality, filters the rolling poly (ether-sulfone) ultrafiltration membrane ultrafiltration that the back adds molecular weight cut-off 6000, sees through liquid and adds molecular weight cut-off 400 rolling polyether sulfone filtering membrane filtrations again, adding rolling polyethersulfone reverse osmosis membrane again through liquid concentrates, concentrated solution is transferred pH10, uses dichloromethane extraction 3 times, and extraction liquid is concentrated into small volume.Get chloroform, ethanol, phosphate sodium dihydrogen buffer solution (pH6), mix standing demix at 3: 4: 2 in proportion, take off and be full of the high speed adverse current chromatogram post phase that fixes mutually, start main frame, adjust rotating speed 1000rpm, pump into phase, treated that liquid flows out, and adjusts flow velocity 1ml/min, there is sampling valve to advance concentrated solution simultaneously, collect target component according to the UV-detector collection of illustrative plates, preparation continuously, the flow point cryodrying gets Tocosamine 43g, detect content 98.1% through HPLC.
Claims (4)
1. the preparation method of a Tocosamine is characterized in that may further comprise the steps:
A. the Herba Thermopsis Lanceolatae seed is pulverized, and adds 0.5-1% hydrochloric acid or aqueous sulfuric acid cold soaking, and extracting solution is regulated the neutral filtration of pH, adds the ultra-filtration membrane ultrafiltration, adds nanofiltration membrane again and filters, and sees through liquid and concentrates with reverse osmosis membrane, gets concentrated solution;
B. above-mentioned concentrated solution is transferred pH9-10, uses dichloromethane extraction, adopts high speed adverse current chromatogram to separate again after extraction liquid concentrates, and collects target component according to the UV-detector collection of illustrative plates, and cryodrying promptly.
2. the preparation method of Tocosamine as claimed in claim 1 is characterized in that the described ultra-filtration membrane molecular weight cut-off of step a 3000-10000, nanofiltration membrane molecular weight cut-off 300-600.
3. the preparation method of Tocosamine as claimed in claim 1, it is characterized in that a kind of in the described ultra-filtration membrane of step a, nanofiltration membrane and the optional tubular type of reverse osmosis membrane, rolling and the hollow membrane, a kind of in the optional tynex of material, polyethersulfone, the tetrafluoroethylene.
4. the preparation method of Tocosamine as claimed in claim 1, it is characterized in that the described high speed adverse current chromatogram solvent systems of step b is chloroform, ethanol, phosphate sodium dihydrogen buffer solution (pH5-6), blending ratio 3-5: 4-5: 2-3, on be moving phase mutually, is stationary phase mutually down.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101515092A CN102219786A (en) | 2011-06-07 | 2011-06-07 | Preparation method of sparteine |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011101515092A CN102219786A (en) | 2011-06-07 | 2011-06-07 | Preparation method of sparteine |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN102219786A true CN102219786A (en) | 2011-10-19 |
Family
ID=44776514
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2011101515092A Pending CN102219786A (en) | 2011-06-07 | 2011-06-07 | Preparation method of sparteine |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102219786A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588773A (en) * | 2013-11-07 | 2014-02-19 | 东南大学 | Method for extracting and separating cytisine |
| CN107847493A (en) * | 2015-07-31 | 2018-03-27 | 阿提努公司 | Antibechic drug composition and method |
| CN109959735A (en) * | 2019-03-29 | 2019-07-02 | 完美（广东）日用品有限公司 | The content assaying method of three kinds of ingredients in line leaf broom top, line leaf goldspink flower extract and line leaf goldspink jasmine tea |
-
2011
- 2011-06-07 CN CN2011101515092A patent/CN102219786A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103588773A (en) * | 2013-11-07 | 2014-02-19 | 东南大学 | Method for extracting and separating cytisine |
| CN103588773B (en) * | 2013-11-07 | 2016-01-06 | 东南大学 | A kind of extraction and separation method of Tocosamine |
| CN107847493A (en) * | 2015-07-31 | 2018-03-27 | 阿提努公司 | Antibechic drug composition and method |
| JP2018522020A (en) * | 2015-07-31 | 2018-08-09 | アテヌア インコーポレイテッド | Antitussive composition and method |
| EP3328383A4 (en) * | 2015-07-31 | 2019-01-16 | Attenua, Inc. | Antitussive compositions and methods |
| CN109959735A (en) * | 2019-03-29 | 2019-07-02 | 完美（广东）日用品有限公司 | The content assaying method of three kinds of ingredients in line leaf broom top, line leaf goldspink flower extract and line leaf goldspink jasmine tea |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN106198172A (en) | A kind of selective enrichment method of tree peony anthocyanins in black Fructus Lycii | |
| CN104892687A (en) | Method for separating and purifying monomeric compound from Chinese mahonia leaves through high-speed counter-current chromatography | |
| CN101016344A (en) | Process of preparing high purity tea polysaccharide | |
| CN101607964B (en) | Preparation method of cycle epimedium aglucone | |
| CN102219786A (en) | Preparation method of sparteine | |
| CN105367531A (en) | Method for separating two homoisoflavonoids in fibrous roots of ophiopogon japonicusby adopting recycling high-speed counter-current chromatography | |
| CN102627679A (en) | Method for preparing schaftoside from desmodium styracifolium | |
| CN108218948A (en) | A kind of preparation method of Sodium Aescinate | |
| CN102898347A (en) | Method for extracting caragana microphylla from hypaphorine | |
| CN112266399A (en) | High-purity separation and extraction method of epimedium extract | |
| CN102260307A (en) | Method for preparing specnuezhenide | |
| CN104262231B (en) | From white thorn seed, extract the method that separates L-Trp | |
| CN103242414B (en) | A kind of method from Stem of Oriental Bittersweet medicinal material separation and purification Tripterine | |
| CN105434539A (en) | Composition of lotus flavones | |
| CN113354697B (en) | Method for separating and purifying pectolinarin and linarin | |
| CN112898258B (en) | Separation preparation method of high-purity hyoscyamine | |
| CN104945355B (en) | The method and system of separation dihydro phaseic acid is extracted from Desmodium styracifolium | |
| CN103435512A (en) | Method for preparing kukoamine B | |
| CN103965276B (en) | The method of fast separating and purifying monomeric compound from Lindley Eupatorium Herb | |
| CN104945391B (en) | The method and system of extraction separation Schaftoside from Desmodium styracifolium | |
| CN107235988A (en) | A kind of extracting method of qinghaosu and Artemisitene | |
| CN102268052A (en) | Method for preparing camellianin A | |
| CN113831313A (en) | Preparation method and application of high-purity coumarin derivative | |
| CN102391344A (en) | Method for preparing picfeltarraenin IA from picria feltarrae lour leaves | |
| CN104610209A (en) | Industrial method for improving purity of barbaloin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20111019 |