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Preparation method of veratrum alkaloid

An alkaloid and veratroline technology, applied in the field of veratroline alkaloid preparation, can solve the problems of low yield, no clear indication of the final product yield, etc., achieve good repeatability, reduce the destruction of product active ingredients and the elimination of by-products. Produce, process safe and reasonable effect

Inactive Publication Date: 2014-01-22
JIANGSU TIANSHENG PHARMA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The content of this patent is to separate and purify two of the many alkaloids in veratrum. Although the yield of the final product is not clearly indicated in the patent, due to the repeated use of steps such as heating, extraction and concentration in the preparation process, the obtained rate will also be low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] (1) Take 5 kg of Veratrum medicinal material, crush it into coarse powder, add 25 L of hydrochloric acid aqueous solution with a pH value of 3.0 to carry out cold extraction, the extraction temperature is 25 ° C, and extract twice, each time for 3 hours.

[0035] (2) Combine the extracts, filter, and add 2% aqueous sodium bicarbonate solution to the filtrate under stirring to adjust the solution to pH to 8.5, then add 15L ethyl acetate for extraction, leave it for 1 hour, and separate the ethyl acetate layer .

[0036](3) Add 5 L of water to ethyl acetate and extract twice, separate and discard the water layer, and take the ethyl acetate layer.

[0037] (4) Add 10 L of hydrochloric acid aqueous solution with a pH value of 6 to ethyl acetate for extraction, let stand, and separate the water layer.

[0038] (5) Take the water layer solution and pass it through the resin column of model D061. After loading the column, add 25 L of water to elute, then use 0.5% sodium hydro...

Embodiment 2

[0042] (1) Take 10 kg of Veratrum medicinal material, crush it into a coarse powder, add 45 L of hydrochloric acid aqueous solution with a pH value of 3.5, and carry out cold-extraction. The extraction temperature is 15° C., and the extraction is performed twice, each time for 2 hours.

[0043] (2) Combine the extracts, filter, and add 1% aqueous sodium hydroxide solution to the filtrate under stirring to adjust the solution to pH to 9.0, then add 30L n-butanol to extract, leave standstill for 2 hours, and take the n-butanol layer .

[0044] (3) Add water to n-butanol and add 10 L of water to extract three times, separate and discard the water layer, and take the n-butanol layer.

[0045] (4) Add 15 L of sulfuric acid aqueous solution with a pH value of 5.5 to the organic layer for extraction, let stand, and separate the water layer.

[0046] (5) Take the water layer solution and pass it through the resin column of model D001SS. After loading the column, add 30L of water to e...

Embodiment 3

[0050] (1) Take 10 kg of Veratrum medicinal material, grind it into coarse powder, add 50 L of sulfuric acid aqueous solution with a pH value of 2.5 to carry out cold extraction, the extraction temperature is 25 ° C, and extract 3 times, each time for 2 hours.

[0051] (2) Combine the extracts, filter, add 0.8% potassium hydroxide aqueous solution to the filtrate under stirring to adjust the solution to pH to 7.5, then add 25L ethyl acetate for extraction, let stand for 2 hours, and separate the ethyl acetate layer .

[0052] (3) Add water to ethyl acetate and add 8 L of water to extract twice, separate and discard the water layer, and take the ethyl acetate layer.

[0053] (4) Add 10 L of sulfuric acid aqueous solution with a pH value of 6.5 to the organic layer for extraction, let stand, and separate the water layer.

[0054] (5) Take the aqueous layer solution and pass it through a resin column of NKC-9 type. After loading the column, add 20 L of water for elution, then us...

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Abstract

The invention provides a preparation method of veratrum alkaloid, and belongs to the field of organic chemistry. The preparation method is as follows: the veratrum alkaloid is prepared through a series of steps of leaching, extraction, column chromatography, crystallization, and the like by taking a veratrum medicinal material as a raw material, and the content of the veratrum alkaloid achieves 80%-98%. The preparation process provided by the invention is safe and reasonable; because a heating procedure is not adopted in the preparation process of the veratrum alkaloid, the condition that the veratrum alkaloid is sufficiently extracted and separated is ensured farthest, and the damage of the active components of a product and the generation of a by-product due to a heating condition are reduced, so that the yield and safety of the product are enhanced. The process provided by the invention has the advantages of good stability and repeatability, controllability in quality and very high practicability through the verification of batched industrialized production.

Description

technical field [0001] The invention relates to a preparation method of veratrum alkaloid with antiviral effect, which belongs to the field of organic chemistry. Background technique [0002] Falsehellebore Root and Rhizome is the dry root and rhizome of the plant Veratrum in the family Liliaceae. First recorded in "Shen Nong's Materia Medica", it is bitter, pungent, cold, and poisonous. Return lung, stomach warp. "Compendium of Materia Medica" is recorded in the Ministry of Grass, poisonous weeds, which have the effects of vomiting wind and phlegm, killing insects and poisoning. [0003] The main chemical component in Veratrum is alkaloids. Due to its strong physiological activity, when its alkaloid components are used in combination with many other traditional Chinese medicines, chemical reactions will occur, and accidents will occur. Therefore, Veratrum has always been known for its high toxicity in traditional Chinese medicine. For example, in the "Eighteen Anti-Songs...

Claims

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Application Information

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IPC IPC(8): A61K36/896A61P31/12
Inventor 杨永安钟慧金显友易铭魏元刚袁继文黄全书季浩
Owner JIANGSU TIANSHENG PHARMA
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