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Process for separating corydalmine alkaloids by utilizing alkaline silica gel

A technology of Corydalis and alkaloids, applied in the field of chemical industry, can solve the problems of large separation limitation, industrialization limitation, sample loss, etc., and achieves the effects of simple process operation, simple and convenient preparation, and reduced production cost.

Inactive Publication Date: 2013-07-24
CHINA PHARM UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it has to be separated at 7°C and has great limitations.
And because Corydalina is easy to form dead adsorption on the silica gel column, it causes serious loss of samples, which is unfavorable for industrialized production
[0005] At present, high-speed countercurrent chromatography is also commonly used in the separation and purification of alkaloids. Compared with traditional methods, the efficiency is greatly improved, and the problem of dead adsorption of alkaloids on the separation medium is solved. However, due to its small sample load, it is difficult to expand its application and economical. The benefit is not high, and the equipment is expensive, so the high-speed countercurrent method for the separation of Corydalis alkaloids has certain limitations for industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Take 2 L of the extract containing Corydalina alkaloid, adjust the pH to 8 with ammonia water, extract 3 times with 2 times the volume of ethyl acetate, combine the extracts, and recover the solvent under reduced pressure to obtain a crude extract. Take 0.75g of crude extract, dissolve it with a small amount of mixed solution of dichloromethane and methanol, add 1.5g of silica gel to mix the sample, evaporate the solvent and load the sample. Take 15 g of alkalized silica gel containing 1% sodium hydroxide mass fraction, and put it in a column with a diameter of 1.6 cm by wet method with petroleum ether to obtain a column layer with a height of 24.5 cm. Gradient elution with petroleum ether-acetone system: first Wash 10BV (column volume) with petroleum ether-acetone (9:1), and then wash 15BV with petroleum ether-acetone (85:15), flow rate 1BV / h. Use thin-layer chromatography to test the fractions, combine the parts containing Corydalis damina, recrystallize with methanol...

Embodiment 2

[0023] Take 0.5g of crude extract containing Corydalina alkaloid, dissolve it in a small amount of methanol, add 1.0g of silica gel to mix the sample, evaporate the solvent and load the sample. Take 15 g of column silica gel with a mass fraction of 0.5% sodium hydroxide, and wet-install it in a column with a diameter of 1.6 cm with petroleum ether to obtain a column layer with a height of 24.5 cm, and then use a petroleum ether-acetone system for pressure gradient elution : First wash 10BV with petroleum ether-acetone (7:1), then rinse 10BV with petroleum ether-acetone (85:15), flow rate 1.5BV / h. Use thin-layer chromatography to test the fractions, combine the parts containing Corydalina, recover the solvent and recrystallize with methanol-water to obtain Corydalamine with a purity of 98.1%, and the recovery rate of Corydalamine alkaloids is 65%. %.

Embodiment 3

[0025] Take 0.38g of the crude extract containing Corydalis alkaloid, dissolve it in a small amount of dichloromethane, add 1.0g of silica gel to mix the sample, evaporate the solvent and load the sample. Take 15 g of column silica gel with a mass fraction of 0.1% sodium hydroxide, and wet-pack it in a column with a diameter of 1.6 cm with petroleum ether to obtain a column layer with a height of 24.5 cm, and then use petroleum ether-acetone (9:1) isocratic Flushing 30BV, flow rate 2.5BV / h. The fractions were tested by thin-layer method, and the fractions containing Corydalamine were combined. After recovering the solvent, recrystallized with methanol-water to obtain Corydalamine with a purity of 98.0%, and the recovery rate of Corydalamine alkaloid was 62%. .

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Abstract

The invention discloses a process for separating corydalmine alkaloids by utilizing alkaline silica gel, relating to the field of chemical industry and specifically relating to the process for separating the corydalmine alkaloids by utilizing the alkaline silica gel to perform chromatography. The process is characterized by comprising the following steps of: dissolving a crude extract containing the corydalmine alkaloids by using an appropriate amount of methylene dichloride and / or methanol, mixing with the alkaline silica gel, then performing column chromatography separation by using the alkaline silica gel, performing elusion with one or more of petroleum ether, acetone, methylene dichloride, water and ammonia water, detecting fractions by thin layer chromatography, and merging the fractions containing corydalmine; and recovering the fractions, performing decompression recovery on the solvent, and performing recrystallization to obtain the corydalmine alkaloids with the purity of more than 98%. The process disclosed by the invention has the advantages of no need of using special filler, simplicity in operation, low sample loss, stability and low cost, and can realize the operation from small-quantity preparation in a laboratory to expanded industrial production so as to reduce the production cost.

Description

technical field [0001] The invention relates to the field of chemical industry, in particular to a process for separating Corydalina alkaloids by alkalized silica gel chromatography. Background technique [0002] Violet Damamine is a benzylisoquinoline alkaloid, a natural trace active ingredient with good analgesic activity, and has the characteristics of high-efficiency and rapid analgesia, but its natural sources are very limited, which limits its application in the pharmaceutical field application. The patent application No. 201110125328 discloses a biotransformation and fermentation process for the efficient production of Corydalis damming, and the yield of Corydalis damming produced by transformation and fermentation reaches more than 50%. [0003] At present, there are many separation methods for alkaloid compounds, such as solvent extraction, distillation, precipitation, salting out, crystallization, etc. There are also more advanced separation methods such as silica...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D455/03
Inventor 刘吉华余伯阳王严
Owner CHINA PHARM UNIV
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