CN102100725B - Preparation technology of extracting total alkaloid extraction from Gansu whin - Google Patents
Preparation technology of extracting total alkaloid extraction from Gansu whin Download PDFInfo
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- CN102100725B CN102100725B CN2009101177525A CN200910117752A CN102100725B CN 102100725 B CN102100725 B CN 102100725B CN 2009101177525 A CN2009101177525 A CN 2009101177525A CN 200910117752 A CN200910117752 A CN 200910117752A CN 102100725 B CN102100725 B CN 102100725B
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- herba oxytropis
- oxytropis kansuensis
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Abstract
The invention discloses a preparation technology of extracting total alkaloid extraction from Gansu whins. In the invention the raw material of Gansu whins is extracted by heating in water, the extract is condensed under a reduced pressure, acidified, and loaded on a cation column for ion exchange adsorption; water and alcohol solution containing water are used to flush the column in order, then the cation column is eluted by an alkaline alcohol solution; and the alkaline alcohol eluate is collected, condensed, and dried to obtain the product. In the invention the production rate of total alkaloid extraction is high; the extraction cost is low; the technology is simple; the preparation process is safe; and the whole extraction technology is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of from Herba Oxytropis Kansuensis the production technology of separation and Extraction total alkaloids extract.
Background technology
Herba Oxytropis Kansuensis (O xy trop is kansuensis) mainly is distributed in pastures, ground such as China Qinghai, Gansu, Ningxia, Sichuan, Yunnan for the pulse family Herba Oxytropis Kansuensis belongs to herbaceos perennial, and output is huge.The research of Herba Oxytropis Kansuensis bioactive ingredients is thought that its contained alkaloid is a main active.Its contained alkaloid is mainly (.+-.)-Swainsonine (swainsonine), thermopsine (thermopsine), sparteine (sparteine), anagyrine (anagyrine) etc.This Alkaloid has many-sided pharmacological actions such as anticancer, anti-heart rate imbalance, antimicrobial, antiulcer, leukocyte increasing.(.+-.)-Swainsonine is a main component in its alkaloid, and (.+-.)-Swainsonine is a western pyridine Alkaloid in a kind of indole of high polarity, and alpha-Mannosidase is had special inhibitory action.(.+-.)-Swainsonine has obtained the concern of domestic and international research worker as a kind of brand-new cancer therapy drug in recent years, and its characteristics are both to have the effect of direct killing tumor cell, have immunoregulatory two-way function again.
Summary of the invention
The object of the present invention is to provide a kind of from Herba Oxytropis Kansuensis the technology of separation and Extraction total alkaloids extract; This process using water is carried; Concentrating under reduced pressure, cation exchange resin column absorption after the acid adjustment property, water, aqueous alcohol solutions are washed remove impurity successively; Alkaline aqueous alcoholic solution eluting is collected the eluent concentrating under reduced pressure and is drying to obtain the Herba Oxytropis Kansuensis total alkaloids extract.
The present invention is with exsiccant Herba Oxytropis Kansuensis raw material; Through the water heating extraction; With the extracting solution concentrating under reduced pressure, acidify, last cation seperation column exchange absorption; The alkaline alcohol solution eluting is used in water and aqueous alcohol liquid flushing back successively, obtains the Herba Oxytropis Kansuensis total alkaloids extract behind the collection alkaline ethanol eluent concentrate drying.
A kind of from Herba Oxytropis Kansuensis the preparation technology of extract total alkaloids extract, it is characterized in that preparation technology is:
A is with exsiccant Herba Oxytropis Kansuensis raw material, and the water logging bubble post-heating that adding 6-12 doubly measures boils and carries 0.5-2h, and extracting solution is inclined to, and repeats to extract for several times; Merge extracting solution for several times, get the Herba Oxytropis Kansuensis extracting solution;
B is evaporated to the Herba Oxytropis Kansuensis aqueous extract and is equivalent to crude drug 0.6-1.0g/ml, gets the Herba Oxytropis Kansuensis concentrated solution;
C uses the dilute acid soln adjust pH to be acidity the Herba Oxytropis Kansuensis concentrated solution, and last cation exchange resin column exchanges absorption, first standing adsorption, and circulation absorption twice then, and adsorption liquid discards;
Cationic resin column to effluent after D adsorbs with the deionized water rinsing exchange is neutral colourless, and eluent discards;
E is faint yellow with ethanol water flushing cationic resin column to effluent, and eluent discards;
F collects eluent with the alcohol-water solution eluting cation seperation column that contains 0.5-4wt% alkali, transfers pH 5-6 with acid behind the concentrating under reduced pressure, obtains the Herba Oxytropis Kansuensis total alkaloids extract then after the drying.
After the resin cation exchange absorption of the present invention, after taking out impurity, use the remove impurity of ethanol water rinse resin again, adopt the alkaline alcohol solution eluting then with the washed with de-ionized water resin.
Yield of extract of the present invention is 0.6～1.0%, and total alkaloid content is greater than 50% in the extractum.
Adopt the present invention to extract that total alkaloids uses solvent safety inexpensive, simple to operate in the Herba Oxytropis Kansuensis, whole technology is easy to realize suitability for industrialized production.
Description of drawings
Fig. 1 is the process flow diagram of extract total alkaloids from Herba Oxytropis Kansuensis.
The specific embodiment
Embodiment 1
Get Herba Oxytropis Kansuensis Radix Glycyrrhizae 1kg, add 12L water logging bubble 0.5h, be heated to boiling then and extract 2h, inclining the supernatant; Add the heating of 10L water again and carry out the extraction second time; Extracted twice liquid is merged, be evaporated to and be equivalent to crude drug 0.6g/mL, with dilute hydrochloric acid adjustment pH value to 1; Last cationic resin column exchange absorption; Treat that medicinal liquid is full of closure piston standing adsorption 2.5h behind the whole resin column, circulation absorption is 2 times then, and flow velocity is 0.7BV/h.Treat absorption finish the back with the deionized water rinsing resin column to neutral and colourless basically, wash pillar to eluent with 70% alcoholic solution then and be faint yellow and stop, eluent discards.Then with the 70% alcoholic solution eluting cation exchange resin column that contains the 1wt% sodium hydroxide; Flow velocity is 0.4BV/h, collects alkaline eluant, takes out behind decompression and solvent recovery to the small size; Transfer the about 5-6 of pH with rare HCl solution; Put into the vacuum drying oven drying under reduced pressure then and promptly get the Herba Oxytropis Kansuensis total alkaloids extract to doing, yield of extract is 0.8%, and total alkaloid content is greater than 56% in the extractum.
Claims (1)
1. the preparation technology of an extract total alkaloids extract from Herba Oxytropis Kansuensis is characterized in that preparation technology is:
A is with exsiccant Herba Oxytropis Kansuensis raw material, and the water logging bubble post-heating that adding 6-12 doubly measures boils and carries 0.5-2h, and extracting solution is inclined to, and repeats to extract for several times; Merge extracting solution for several times, get the Herba Oxytropis Kansuensis extracting solution;
B is evaporated to the Herba Oxytropis Kansuensis aqueous extract and is equivalent to crude drug 0.6-1.0g/ml, gets the Herba Oxytropis Kansuensis concentrated solution;
C uses the dilute acid soln adjust pH to be acidity the Herba Oxytropis Kansuensis concentrated solution, and last cation exchange resin column exchanges absorption, first standing adsorption, and circulation absorption twice then, and adsorption liquid discards;
Cationic resin column to effluent after D adsorbs with the deionized water rinsing exchange is neutral colourless, and eluent discards;
E is faint yellow with 70% ethanol water flushing cationic resin column to effluent, and eluent discards;
F collects eluent with the 70% ethanol aqueous wash decationized Y sieve post that contains 0.5-4wt% alkali, transfers pH 5-6 with acid behind the concentrating under reduced pressure, obtains the Herba Oxytropis Kansuensis total alkaloids extract then after the drying.
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101177525A CN102100725B (en) | 2009-12-18 | 2009-12-18 | Preparation technology of extracting total alkaloid extraction from Gansu whin |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2009101177525A CN102100725B (en) | 2009-12-18 | 2009-12-18 | Preparation technology of extracting total alkaloid extraction from Gansu whin |
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| CN102100725A CN102100725A (en) | 2011-06-22 |
| CN102100725B true CN102100725B (en) | 2012-05-09 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103073544B (en) * | 2011-10-25 | 2014-12-24 | 中国科学院兰州化学物理研究所 | Method for separating swainsonine by using counter-current chromatography |
| CN105481921B (en) * | 2015-12-29 | 2018-04-06 | 中国科学院西北高原生物研究所 | Compound method in chromatographic isolation whin is prepared based on parallel clastotype |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177426A (en) * | 2006-11-11 | 2008-05-14 | 中国科学院兰州化学物理研究所 | Process for separating extracting spherosinin from gansu whin |
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- 2009-12-18 CN CN2009101177525A patent/CN102100725B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101177426A (en) * | 2006-11-11 | 2008-05-14 | 中国科学院兰州化学物理研究所 | Process for separating extracting spherosinin from gansu whin |
Non-Patent Citations (3)
| Title |
|---|
| 王明娟等.甘肃棘豆生物碱部位体内抗肿瘤作用及对免疫功能的影响.《中国中西医结合杂志》.2009,第29卷(第11期),1009-1011. * |
| 石勇等.疯草毒性成分苦马豆素的研究概况.《中药处》.1999,第22卷(第1期),47-49. * |
| 赵宝玉等.甘肃棘豆_Oxytropiskansuensis_毒性生物碱研究.《中国兽医学报》.2001,第21卷(第2期),174-176. * |
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| CN102100725A (en) | 2011-06-22 |
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