Method for separating and preparing rumicin

A technology of ruminoid and high-speed countercurrent chromatography, which is applied in the field of high-speed countercurrent chromatography to separate and prepare high-purity ruminoid, and achieves the effects of short time, mild conditions and high recovery rate

Inactive Publication Date: 2012-05-30
苏州宝泽堂医药科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This technology does not use solid adsorbents, it is an all-liquid chromatography method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Take 150 g of Radix Hibiscus (manufactured in Nanjing), infiltrate with 100 ml of dichloromethane, and extract by percolation until the color of the percolation liquid becomes lighter, and recover the solvent to obtain 16.3 g of a brown crude dry product.

[0020] A high-speed countercurrent chromatograph is used, and the chromatographic separation solvent system is composed of petroleum ether-ethyl acetate-ethanol-water, and the volume ratio is 6:8:4:2. Set layering, take the upper phase as the stationary phase, and the lower phase as the mobile phase, take 1.5 g of the crudely extracted dry matter and dissolve it in the mixed solvent of the upper and lower layers of 30 ml, so that the column of the high-speed countercurrent chromatography is filled with the stationary phase, and then the column The head end is connected with the injection valve, and the speed controller is turned on to make the host rotate until the rotation speed reaches 700rpm, and the mobile phase i...

Embodiment 2

[0022] Take 150 g of Radix Hibiscus (manufactured in Nanjing), infiltrate with 100 ml of dichloromethane, and extract by percolation until the color of the percolation liquid becomes lighter, and recover the solvent to obtain 16.3 g of a brown crude dry product.

[0023] A high-speed countercurrent chromatograph is used, and the chromatographic separation solvent system is composed of petroleum ether-ethyl acetate-ethanol-water, and the volume ratio is 8:10:6:4. The solvent system is arranged in a separatory funnel, fully shaken and static Set layering, take the upper phase as the stationary phase, and the lower phase as the mobile phase, get 2.1 g of the crudely extracted dry matter and dissolve it in the mixed solvent of 40 ml upper and lower layers, so that the column of the high-speed countercurrent chromatograph is filled with the stationary phase, and then the column The head end is connected with the injection valve, and the speed controller is turned on to make the host...

Embodiment 3

[0025] Take 150 g of Radix Hibiscus (manufactured in Nanjing), infiltrate with 100 ml of dichloromethane, and extract by percolation until the color of the percolation liquid becomes lighter, and recover the solvent to obtain 16.3 g of a brown crude dry product.

[0026] A high-speed countercurrent chromatograph is used, and the chromatographic separation solvent system is composed of petroleum ether-ethyl acetate-ethanol-water, and the volume ratio is 5:7:5:3. Place layers, take the upper phase as the stationary phase, and the lower phase as the mobile phase, get 2.5 g of the crudely extracted dry matter and dissolve it in the mixed solvent of the upper and lower layers of 50 ml, so that the column of the high-speed countercurrent chromatography is filled with the stationary phase, and then the column The head end is connected with the injection valve, and the speed controller is turned on to make the host rotate until the rotation speed reaches 900rpm, and the mobile phase is...

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PUM

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Abstract

The present invention discloses a method for separating and preparing rumicin. The method comprises subjecting sheep hooves to percolation extraction with dichloromethane, and recovering the solvent to obtain a dry crude extract; and selecting a two-phase solvent system, adopting high-speed countercurrent chromatography, dissolving the crude extract in a mixed solution of a top phase and a bottom phase, filling a stationary phase in a separation column, connecting the head end of the separation column with a sampling valve, collecting an isolate, concentrating, and drying to obtain the final product. The two-phase solvent system is a petroleum ether-ethyl acetate-ethanol-water system, the top phase is the stationary phase, and the bottom phase is a mobile phase. The prepared product has content of rumicin up to 98%.

Description

Technical field: [0001] The invention relates to a method for separating and preparing high-purity sorrel by high-speed countercurrent chromatography (HSCCC). Background technique: [0002] Rumex japonicus Houtt. is a plant of the genus Rumex in the family Polygonaceae, also known as Rumex, Jinbuhuan, etc. It is a perennial herb with extremely rich resources. It is widely distributed in East China, Central China, and South China. It is born in fields, roadsides, River beaches, ditch edge wetlands. Its roots are used as medicine, and it is a commonly used medicine. It was first recorded in "Shen Nong's Materia Medica", and it was listed as a low-grade product. It tastes bitter and cold in nature. It has the effects of killing insects, promoting blood circulation and stopping bleeding, clearing heat and detoxifying, and is used for skin diseases, scabies, various bleeding and various inflammations. Yuanyuan et al. used high performance liquid chromatography to determine the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C49/83C07C45/79
Inventor 李法庆刘东锋
Owner 苏州宝泽堂医药科技有限公司
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