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Method for preparing high-purity veratramine and jervine

A technology of mesphenamine and veratramine, which is applied in the field of preparing high-purity veratramine and mesphenamine, can solve the problems of low yield, high production cost, and high organic solvent residue, and achieve high yield, simple operation, The effect of high degree of automation

Inactive Publication Date: 2012-05-30
SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, in terms of the preparation of veratrol steroidal alkaloids, there are no reports on the industrial preparation of high-purity veratramine and mephenamine at home and abroad.
And laboratory research report, the preparation method of veratrol steroidal alkaloid mainly contains after alcohol extraction, acid water dissolution, alkali precipitation method, adopts this method, the loss of veratrol steroidal alkaloid is very large, and yield is low, and production cost Another method is to use alcoholic organic solvents to extract, after concentration, extract and enrich with organic solvents of different polarities, such as chloroform, dichloromethane, ethyl acetate, etc., but using this method, the residual organic solvents are high, Disadvantages such as high toxicity, complicated operation steps, high impurity content, and unsuitable for industrial production operations

Method used

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  • Method for preparing high-purity veratramine and jervine
  • Method for preparing high-purity veratramine and jervine
  • Method for preparing high-purity veratramine and jervine

Examples

Experimental program
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Effect test

Embodiment 1

[0021] Preparation of high-purity Veratramine (Veratramine) and Jervine (Jervine) After 5Kg of Veratrum medicinal material is pulverized, it is extracted three times with 60% ethanol under reflux in an atmospheric extraction device, each time for 1 hour, and the extract is filtered and concentrated under reduced pressure to No alcohol smell, the concentrated solution is diluted with 2 times the volume of water and diluted with water, then added to the AB-8 macroporous adsorption resin column, eluted with 150L of deionized distilled water, and then eluted with 100L of 0.05% sodium hydroxide aqueous solution , followed by elution with 100L of 10-60% ethanol solution for decolorization, and then eluting veratrum alkaloid components with 70-90% alcohol. After mixing, carry out silica gel column chromatography, elute with petroleum ether: ethyl acetate 2: 1 ~ 1: 2 mobile phase, thin-layer chromatography tracking, collect veratramine and mephenamine respectively, and the collected so...

Embodiment 2

[0023] After 5Kg of Veratrum medicinal material is pulverized, extract three times with 75% ethanol under reflux in an atmospheric extraction device, each time for 2 hours, the extract is filtered and concentrated under reduced pressure until there is no alcohol smell, diluted with 4 times the volume of the concentrated solution and diluted with water, added On the D101 macroporous adsorption resin column, elute with 150L of deionized distilled water, then with 100L of 0.1% potassium hydroxide aqueous solution, then with 100L of 10-60% ethanol solution for decolorization, and then with 70-90% alcohol elutes the veratrum alkaloid components, and the eluent is concentrated under reduced pressure until it has no alcohol smell. After mixing with 250g alumina, carry out alumina column chromatography, using petroleum ether: ethyl acetate: Methanol: ammonia water 7:5:1:0.1~3:5:1:0.1 Elution, TLC tracking, respectively collect veratramine and mephenamine, the collected solution was con...

Embodiment 3

[0025] After 10Kg of Veratrum medicinal material is pulverized, it is extracted three times with 90% ethanol in an atmospheric extraction device under reflux, each time for 3 hours, and the extract is filtered and concentrated under reduced pressure until it has no alcohol smell. ZTC-1 macroporous adsorption resin column, eluted with 300L of deionized distilled water, then eluted with 200L of 0.5% calcium hydroxide aqueous solution, followed by elution with 200L of 10-60% ethanol solution for decolorization, Then elute the Veratrum alkaloid components with 70-90% alcohol, concentrate the eluent under reduced pressure to no alcohol smell, mix with 400g reversed-phase silica gel, carry out reversed-phase silica gel column chromatography, and use methanol: water Eluted at 50:50~70:30, tracked by thin layer chromatography, collected veratramine and mephenamine respectively, the collected solution was concentrated to dryness under reduced pressure, then recrystallized in methanol so...

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Abstract

The invention provides a method for preparing high-purity veratramine and jervine. The method comprises the steps of: crashing crude veratrum drugs, distilling and extracting alcohol, enriching, eluting (desorbing) and concentrating macroporous absorbent resin, then obtaining veratrum steroid alkaloid, conducting column chromatography purification and recrystalization, drying and obtaining the finished product of monomer. The purity of the veratramine and jervine prepared in the method can reach above 90 percent. The method for preparing high-purity veratramine and jervine has simple process and high yield, and is suitable for industrialized production.

Description

Technical field: [0001] The present invention relates to medicinal chemistry. Specifically, it relates to a method for preparing high-purity veratramine (Veratramine) and mephenamine (Jervine) by taking veratrum, a traditional Chinese medicinal material, as a raw material. Background technique: [0002] Veratrum (Veratrum Linn.) is a plant of Liliaceae (Liliaceae), and there are about 40 species in the world. According to "Flora of China", there are 13 species and one variety in China. The roots and rhizomes of veratrum are used in traditional Chinese medicine for apoplexy, phlegm congestion, epilepsy, sore throat obstruction, scabies and malignant sores. Phytochemical constituents of Veratrum include steroidal alkaloids, stilbene compounds, dipeptides, flavonoids and other compounds. Among them, alkaloids are the main active ingredients. Modern studies have shown that Veratrum has the effects of lowering blood pressure and anti-tumor, among which Veratrum steroidal alkal...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07J69/00C07J75/00A61P9/12A61P35/00
Inventor 张卫东李慧粱汤建单磊苏娟柳润辉沈云亨徐希科
Owner SECOND MILITARY MEDICAL UNIV OF THE PEOPLES LIBERATION ARMY
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