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Fine purification preparation process for kuh-seng native

A production process and a technology for matrine, which are applied in the field of refining matrine, can solve the problems of excess impurities in the finished product, the purity cannot reach the preparation, and the detection method is insensitive, and achieve the effects of improving the net content and eliminating impurities.

Inactive Publication Date: 2008-12-10
HARBIN ZHENBAO PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the purity of the currently commercially available matrine raw materials is marked as not less than 98.0%, because the inspection of related substances uses thin-layer chromatography, the detection method itself is not sensitive, and the actual purity cannot meet the requirements of the preparation. Finally, the finished product produced by it is unqualified due to excessive impurities

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0008] The refining process of embodiment 1 matrine

[0009] Take oxymatrine, add an equal amount of water to dissolve it, put it on a macroporous adsorption resin column, and elute it with ammonia water with a pH value of 10 until there is no alkaloid reaction, collect the eluate, concentrate, and add 30% hydrogen peroxide to carry out Oxidation, after the reaction is complete, add 40% sodium hydroxide solution to adjust the pH value to 10.5, extract 4 times with chloroform, combine the chloroform layers, concentrate, then add 5 times the amount of ether, let stand for 1 hour, filter, and reduce pressure Drying; reflux with acetone to dissolve the precipitate, filter, stand for crystallization, and then recrystallize with acetone to obtain the white matrine product.

Embodiment 2

[0010] The refining process of embodiment 2 matrine

[0011] Take oxymatrine, add 2 times the amount of water to dissolve it, put it on a macroporous adsorption resin column, and elute it with ammonia water with a pH value of 11 until there is no alkaloid reaction, collect the eluate, concentrate, and add 20% hydrogen peroxide to carry out Oxidation, after the reaction is complete, add 20% sodium hydroxide solution to adjust the pH value to 11, extract 3 times with chloroform, combine the chloroform layers, concentrate, then add 10 times the amount of ether, let stand for 2 hours, filter, and reduce pressure Drying; reflux with acetone to dissolve the precipitate, filter, stand for crystallization, and then recrystallize with acetone to obtain the white matrine product.

Embodiment 3

[0012] The refining process of embodiment 3 matrine

[0013] Take oxymatrine, add 3 times the amount of water to dissolve it, put it on a macroporous adsorption resin column, and elute it with ammonia water with a pH value of 10.5 until there is no alkaloid reaction, collect the eluate, concentrate, and add 10% hydrogen peroxide to carry out Oxidation, after the reaction is complete, add 30% sodium hydroxide solution to adjust the pH value to 10, extract 5 times with chloroform, combine the chloroform layers, concentrate, then add 8 times the amount of ether, let stand for 0.5 hours, filter, and decompress Drying; reflux with acetone to dissolve the precipitate, filter, let stand to analyze the product, and then recrystallize with acetone to obtain the white matrine product.

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PUM

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Abstract

The invention provides a method for refining matrine. The method comprises the following steps of elution on a column, oxidation, extraction, condensation, precipitation, recrystallization, etc; the refining method can better remove impurities; the produced matrine has high purity; the net content of oxymatrine is higher; and the application of the matrine is safer.

Description

technical field [0001] The invention relates to a refining process of matrine. Background technique [0002] Matrine is a mixed base of oxymatrine (Oxymatrine) and a very small amount of oxysophocarpine (Oxysophocarpine). Although the purity of the currently commercially available matrine raw materials is marked as not less than 98.0%, because the inspection of related substances uses thin-layer chromatography, the detection method itself is not sensitive, and the actual purity cannot meet the requirements of the preparation. Ultimately, the finished product produced by it is unqualified due to excessive impurities. Contents of the invention [0003] The object of the present invention is to provide a kind of production technology of refined matrine in view of above-mentioned deficiencies. [0004] In order to achieve the purpose of the present invention, the refined production process of the present invention includes the following steps: dissolve oxymatrine with water,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D471/22C07D455/00
Inventor 方同华
Owner HARBIN ZHENBAO PHARMA
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