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Industrialized preparation method for gelsemium alkaloids directed at koumine preparation

A technology of Gelkins alkaloids and Gelkinsin, which is applied in the field of preparation of Gelkins alkaloids extracts, can solve the problems of low extraction efficiency of water decoction, and achieve the effect of simple process

Inactive Publication Date: 2018-05-04
FUJIAN MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The extraction efficiency of water decoction is low, and the product obtained by this method is the total extract of gynecine alkaloids

Method used

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  • Industrialized preparation method for gelsemium alkaloids directed at koumine preparation
  • Industrialized preparation method for gelsemium alkaloids directed at koumine preparation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The herb was dried at 60°C, crushed through a 60-mesh sieve, added with 95% ethanol and heated under reflux for extraction, the extraction time was 1-3 h, and the filtrate was collected; the extraction was repeated 1-3 times, the combined filtrate was concentrated under reduced pressure, and the ethanol was recovered to There is no alcohol smell, and the crude extract is obtained. The high performance liquid chromatogram of the crude extract is shown in figure 1 . Add 0.2mol / L sulfuric acid to the obtained crude extract to adjust the pH to 2, filter; add sulfuric acid solution (pH = 2) to dissolve the precipitate, filter, operate 1-2 times, and combine the filtrate; add 5 wt % hydroxide Adjust the pH to 12 with sodium, and prepare a sample solution with a concentration of 1.0 g crude drug / mL.

[0037] At room temperature, the sample solution with a concentration of 3 BV of 1.0 g crude drug / mL was passed through a chromatographic column equipped with pretreated HPD-700...

Embodiment 2

[0039]Gelkins medicinal materials were dried at 60°C, crushed through a 60-mesh sieve, added ethanol with a volume concentration of 95% and heated under reflux for extraction for 1-3 hours, and the filtrate was collected; the extraction was repeated 1-3 times, the filtrate was combined, concentrated under reduced pressure, and the ethanol was recovered to No mellow smell, a crude extract is obtained. Add 0.2mol / L sulfuric acid to the obtained crude extract to adjust the pH to 2, filter; add sulfuric acid solution (pH=2) to dissolve the precipitate, filter, operate 1-2 times, combine the filtrate; add 5wt% sodium hydroxide Adjust the pH to 12, and prepare a sample solution with a concentration of 1.0 g crude drug / mL.

[0040] At room temperature, the sample solution with a concentration of 3 BV of 1.0 g crude drug / mL was passed through a chromatographic column equipped with pretreated HPD-700 macroporous adsorption resin at a flow rate of 3 BV / h for adsorption and separation un...

Embodiment 3

[0042] The herb was dried at 60°C, crushed through a 60-mesh sieve, added with 95% ethanol and heated under reflux for extraction, the extraction time was 1-3 h, and the filtrate was collected; the extraction was repeated 1-3 times, the combined filtrate was concentrated under reduced pressure, and the ethanol was recovered to No mellow smell, a crude extract is obtained. Add 0.2mol / L sulfuric acid to the obtained crude extract to adjust the pH to 2, filter; add sulfuric acid solution (pH=2) to dissolve the precipitate, filter, operate 1-2 times, combine the filtrate; add 5wt% sodium hydroxide Adjust the pH to 12, and prepare a sample solution with a concentration of 1.0 g crude drug / mL.

[0043] At room temperature, the sample solution with a concentration of 3 BV of 1.0 g crude drug / mL was passed through a chromatographic column equipped with pretreated HPD-700 macroporous adsorption resin at a flow rate of 3 BV / h for adsorption and separation until the adsorption was satura...

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Abstract

The invention discloses an industrialized preparation method for gelsemium alkaloids directed at koumine preparation. The method comprises the following steps: whole herb of Gelsemium elegans is subjected to heating reflux extraction with ethanol, and a crude extract liquid is obtained; sulfuric acid or hydrochloric acid is added to the crude extract liquid to regulate pH to 2-5, and the mixture is filtered; a sulfuric acid or hydrochloric acid aqueous solution with pH being 2-5 is added to precipitates for dissolution, filtering is performed, and acid and water filtrates are mixed; pH of themixture of the acid and water filtrates is regulated to 8-13, and a loading buffer containing 0.25-1.25 g of crude drug per milliliter is prepared from the mixture; the loading buffer passes through pretreated macroporous adsorption resin for adsorption, the flow rate of the loading buffer is 1-4 BV / h, a resin column is subjected to gradient elution with pure water and ethanol with volume concentration being 10%-90% after adsorption equilibrium, an eluate is detected by bismuth potassium iodide, the positively reacted eluate is collected and subjected to reduced-pressure evaporation to dryness, and gelsemium alkaloid extract containing higher-purity koumine is obtained. The method has the good characteristics of adopting a simple process, being economical and environmentally friendly and the like.

Description

technical field [0001] The invention relates to the technical field of industrial preparation of medicinal plant alkaloids, in particular to a method for preparing an alkaloid extract from an alkaloid plant oriented towards the preparation of a kezin. Background technique [0002] hook kiss ( Gelsemium elegans Benth.) is an evergreen woody vine belonging to the genus of Strychtenaceae. The whole plant is used as medicine, which has the effects of "reducing swelling and pain, dispelling wind and blood stasis, attacking poison and killing insects". The main active ingredients of Gelkins are indole alkaloids, which have pharmacological effects such as anti-inflammatory and analgesic, anti-tumor, anti-psoriasis, and promoting the growth of poultry and livestock. Gelkins alkaloids include nearly 100 kinds of monomers such as keloids, jia, yin, and jiu. In recent years, a series of studies have found that kelezin has significant analgesic and anti-anxiety effects, and has a goo...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D491/22C07G5/00
CPCC07D491/22C07G5/00
Inventor 俞昌喜许盈石冬梅苏燕评何灿强游文兵
Owner FUJIAN MEDICAL UNIV