CN102432606A - Preparation method of antofine - Google Patents
Preparation method of antofine Download PDFInfo
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- CN102432606A CN102432606A CN2011103037057A CN201110303705A CN102432606A CN 102432606 A CN102432606 A CN 102432606A CN 2011103037057 A CN2011103037057 A CN 2011103037057A CN 201110303705 A CN201110303705 A CN 201110303705A CN 102432606 A CN102432606 A CN 102432606A
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- antofine
- extraction
- chloroform
- preparation
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Abstract
The invention provides a preparation method of antofine. The preparation method of antofine comprises the following steps of adding alkaline alcohol into raw material fine powder for infiltration lasting for 2 to 6 hours, putting the mixture of the alkaline alcohol and the raw material fine powder into an extraction tank, carrying out supercritical CO2 extraction, dissolving the extract by 3% of a hydrochloric acid aqueous solution, filtering, carrying out extraction of the filtrate by chloroform, collecting a chloroform layer, recovering chloroform, drying to obtain a crude product, separating antofine from the crude product by a high-speed countercurrent chromatography in the presence of a solvent system comprising hexane, chloroform, methanol and ammonia water having a pH of 8.5, collecting desired components, concentrating, and drying to obtain high-content antofine. The preparation method of antofine has simple processes and produces low pollution. Antofine obtained by the preparation method has high product purity and can realize industrialization enlargement easily.
Description
Technical field
The present invention relates to a kind of preparation method of antofine, particularly relate to a kind of application supercritical CO
2Extraction and high speed adverse current chromatogram prepare the method for antofine.
Background technology
Cynanchum Komarrivii AI Iijiniski is an Asclepiadaceae Cynanchum plant, another name OX-heart Piao, among the people have medicinal, with all herbal medicine, have invigorate blood circulation, effects such as pain relieving, anti-inflammatory.
Antofine is its main active ingredient, is isoquinoline alkaloid.Antofine has stronger cytotoxic activity to K-562, HL-60 and Hela cell, when concentration is 1mg/ml, is 73.1% to the P388 inhibiting rate.Antofine has anti-microbial effect, and Bacillus subtilus, micrococcus luteus and intestinal bacteria etc. are all had remarkable restraining effect.
Through the document retrieval, do not find the relevant report of the industrial extracting and purifying method of antofine as yet.
Summary of the invention
The technical problem that the present invention will solve provides a kind of preparation method of antofine, and this method product yield is high, content is high.
In order to solve the problems of the technologies described above, technical scheme of the present invention is following:
A kind of preparation method of antofine is characterized in that may further comprise the steps:
(1) gets Cynanchum Komarrivii AI Iijiniski raw material fine powder, add alkaline alcohol and soaked into 2-6 hour, add in the extraction kettle, adopt supercritical CO
2Extraction;
(2) extract filters with the dissolving of 3% aqueous hydrochloric acid, and filtrating use chloroform extraction, gets chloroform layer, and recovery chloroform drying obtains bullion;
(3) ammonia soln with normal hexane-chloroform-methanol-pH=8.5 is a solvent systems, adopts high-speed counter-current chromatograph to separate the antofine in the bullion, collects target components, concentrates, is drying to obtain the high-content antofine.
Said step (1) neutral and alkali alcohol is 90-99% methyl alcohol, and ammoniacal liquor is regulated pH8-10.
Supercritical CO in the said step (1)
2Extraction conditions is: extraction temperature is 40-55 ℃, and extracting pressure is 30-40MPa, CO
2Flow is 2-5ml/g crude drug/min, and the extraction time is 2-4h, and separating still I temperature is 40-45 ℃, and pressure is 7-9MPa, and separating still II temperature is 30-40 ℃, and pressure is 4-6MPa.
The ammonia soln volume of normal hexane-chloroform-methanol in the said step (3)-pH=8.5 is 3-5:7-9:4-5:2-4.
Being moving phase mutually on the solvent systems in the said step (3), is stationary phase down mutually.
Positively effect of the present invention is:
1) adopts supercritical CO
2Extraction, environment friendly and pollution-free, efficient is high, and energy consumption is lower;
2) adopt high speed adverse current chromatogram to separate, preparation amount is big, and sample loss is few, and preparation cycle is short, and product content is high.
To combine embodiment to further specify the present invention below, but the scope that the present invention requires to protect is not limited to following embodiment.
Embodiment
Embodiment 1:
Get raw material fine powder 1kg, 90% methyl alcohol that adds 300mlpH10 soaked into 4 hours, added in the extraction kettle and carried out supercritical extraction, and extraction temperature is 55 ℃, and extracting pressure is 32MPa, CO
2Flow is 3ml/g crude drug/min, and the extraction time is 4h, and separating still I temperature is 42 ℃; Pressure is 7MPa, and separating still II temperature is 35 ℃, and pressure is 5MPa; Collect and resolve extract, the aqueous hydrochloric acid dissolution extraction thing with 3% filters; Filtrating is used chloroform extraction, gets chloroform layer, reclaims the chloroform drying and obtains bullion; Get the ammonia soln of normal hexane, chloroform, methyl alcohol, pH=8.5, for 3:7:4:3 mixes, leave standstill by volume, tell phase up and down; Below be stationary phase mutually, on be moving phase mutually, open high-speed counter-current chromatograph, regulate speed adjustment 750rpm; Get phased soln throw out injecting chromatograph, the control flow rate of mobile phase is 2ml/min, collects the antofine flow point; Concentrated, the dry antofine 191mg that gets detects through HPLC, and content is 96.3%.
Embodiment 2:
Get raw material fine powder 1kg, 95% methyl alcohol that adds 400mlpH9 soaked into 6 hours, added in the extraction kettle and carried out supercritical extraction, and extraction temperature is 50 ℃, and extracting pressure is 35MPa, CO
2Flow is 4ml/g crude drug/min, and the extraction time is 3h, and separating still I temperature is 40 ℃; Pressure is 8MPa, and separating still II temperature is 30 ℃, and pressure is 6MPa; Collect and resolve extract, the aqueous hydrochloric acid dissolution extraction thing with 3% filters; Filtrating is used chloroform extraction, gets chloroform layer, reclaims the chloroform drying and obtains bullion; Get the ammonia soln of normal hexane, chloroform, methyl alcohol, pH=8.5, for 4:9:5:2 mixes, leave standstill by volume, tell phase up and down; Below be stationary phase mutually, on be moving phase mutually, open high-speed counter-current chromatograph, regulate speed adjustment 800rpm; Get phased soln throw out injecting chromatograph, the control flow rate of mobile phase is 2.5ml/min, collects the antofine flow point; Concentrated, the dry antofine 230mg that gets detects through HPLC, and content is 95.4%.
Embodiment 3:
Get raw material fine powder 3kg, 99% methyl alcohol that adds 1000mlpH8 soaked into 6 hours, added in the extraction kettle and carried out supercritical extraction, and extraction temperature is 45 ℃, and extracting pressure is 30MPa, CO
2Flow is 2ml/g crude drug/min, and the extraction time is 2h, and separating still I temperature is 40 ℃; Pressure is 7MPa, and separating still II temperature is 35 ℃, and pressure is 5MPa; Collect and resolve extract, the aqueous hydrochloric acid dissolution extraction thing with 3% filters; Filtrating is used chloroform extraction, gets chloroform layer, reclaims the chloroform drying and obtains bullion; Get the ammonia soln of normal hexane, chloroform, methyl alcohol, pH=8.5, for 3:8:5:4 mixes, leave standstill by volume, tell phase up and down; Below be stationary phase mutually, on be moving phase mutually, open high-speed counter-current chromatograph, regulate speed adjustment 700rpm; Get phased soln throw out injecting chromatograph, the control flow rate of mobile phase is 2ml/min, collects the antofine flow point; Concentrated, the dry antofine 601mg that gets detects through HPLC, and content is 95.7%.
Embodiment 4:
Get raw material fine powder 5kg, 99% methyl alcohol that adds 1.8LpH10 soaked into 2 hours, added in the extraction kettle and carried out supercritical extraction, and extraction temperature is 55 ℃, and extracting pressure is 40MPa, CO
2Flow is 5ml/g crude drug/min, and the extraction time is 3h, and separating still I temperature is 45 ℃; Pressure is 8MPa, and separating still II temperature is 40 ℃, and pressure is 4MPa; Collect and resolve extract, the aqueous hydrochloric acid dissolution extraction thing with 3% filters; Filtrating is used chloroform extraction, gets chloroform layer, reclaims the chloroform drying and obtains bullion; Get the ammonia soln of normal hexane, chloroform, methyl alcohol, pH=8.5, for 3:8:5:4 mixes, leave standstill by volume, tell phase up and down; Below be stationary phase mutually, on be moving phase mutually, open high-speed counter-current chromatograph, regulate speed adjustment 900rpm; Get phased soln throw out injecting chromatograph, the control flow rate of mobile phase is 2.5ml/min, collects the antofine flow point; Concentrated, the dry antofine 897mg that gets detects through HPLC, and content is 91.8%.
Embodiment 5:
Get raw material fine powder 10kg, 95% methyl alcohol that adds 3LpH8 soaked into 5 hours, added in the extraction kettle and carried out supercritical extraction, and extraction temperature is 40 ℃, and extracting pressure is 35MPa, CO
2Flow is 3ml/g crude drug/min, and the extraction time is 4h, and separating still I temperature is 40 ℃; Pressure is 8MPa, and separating still II temperature is 30 ℃, and pressure is 6MPa; Collect and resolve extract, the aqueous hydrochloric acid dissolution extraction thing with 2% filters; Filtrating is used chloroform extraction, gets chloroform layer, reclaims the chloroform drying and obtains bullion; Get the ammonia soln of normal hexane, chloroform, methyl alcohol, pH=8.5, for 5:8:5:4 mixes, leave standstill by volume, tell phase up and down; Below be stationary phase mutually, on be moving phase mutually, open high-speed counter-current chromatograph, regulate speed adjustment 850rpm; Get phased soln throw out injecting chromatograph, the control flow rate of mobile phase is 3ml/min, collects the antofine flow point; Concentrated, the dry antofine 2.1g that gets detects through HPLC, and content is 96.0%.
Claims (5)
1. the preparation method of an antofine is characterized in that may further comprise the steps:
(1) gets Cynanchum Komarrivii AI Iijiniski raw material fine powder, add alkaline alcohol and soaked into 2-6 hour, add in the extraction kettle, adopt supercritical CO
2Extraction;
(2) extract filters with the dissolving of 3% aqueous hydrochloric acid, and filtrating use chloroform extraction, gets chloroform layer, and recovery chloroform drying obtains bullion;
(3) ammonia soln with normal hexane-chloroform-methanol-pH=8.5 is a solvent systems, adopts high-speed counter-current chromatograph to separate the antofine in the bullion, collects target components, concentrates, is drying to obtain the high-content antofine.
2. according to the preparation method of the said a kind of antofine of claim 1, it is characterized in that said step (1) neutral and alkali alcohol is 90-99% methyl alcohol, ammoniacal liquor is regulated pH8-10.
3. according to the preparation method of the said a kind of antofine of claim 1, it is characterized in that supercritical CO in the said step (1)
2Extraction conditions is: extraction temperature is 40-55 ℃, and extracting pressure is 30-40MPa, CO
2Flow is 2-5ml/g crude drug/min, and the extraction time is 2-4h, and separating still I temperature is 40-45 ℃, and pressure is 7-9MPa, and separating still II temperature is 30-40 ℃, and pressure is 4-6MPa.
4. according to the preparation method of the said a kind of antofine of claim 1, it is characterized in that the ammonia soln volume of normal hexane-chloroform-methanol in the said step (3)-pH=8.5 is 3-5:7-9:4-5:2-4.
5. according to the preparation method of the said a kind of antofine of claim 1, it is characterized in that being moving phase in the said step (3) on the solvent systems mutually, is stationary phase down mutually.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103037057A CN102432606A (en) | 2011-10-10 | 2011-10-10 | Preparation method of antofine |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2011103037057A CN102432606A (en) | 2011-10-10 | 2011-10-10 | Preparation method of antofine |
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| CN102432606A true CN102432606A (en) | 2012-05-02 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827243A (en) * | 2012-09-20 | 2012-12-19 | 南京泽朗农业发展有限公司 | Method for purifying sakura saponins |
| CN103446211A (en) * | 2013-09-24 | 2013-12-18 | 兰州理工大学 | Cynanchum komarovii total alkaloid and preparing method and application thereof |
-
2011
- 2011-10-10 CN CN2011103037057A patent/CN102432606A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102827243A (en) * | 2012-09-20 | 2012-12-19 | 南京泽朗农业发展有限公司 | Method for purifying sakura saponins |
| CN103446211A (en) * | 2013-09-24 | 2013-12-18 | 兰州理工大学 | Cynanchum komarovii total alkaloid and preparing method and application thereof |
| CN103446211B (en) * | 2013-09-24 | 2016-02-10 | 兰州理工大学 | A kind of Cynanchum Komarovii total alkaloids and its preparation method and application |
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Application publication date: 20120502 |