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Method for separating and preparing ricinine

A technology of ricinine and castor, which is applied in the field of separation and preparation of ricinine, can solve the problems of low purity of ricinine, troublesome crystallization process, small preparation amount, etc., and achieve strong separation ability, short separation time, advanced The effect of large sample volume

Active Publication Date: 2009-09-30
FEED RESEARCH INSTITUTE CHINESE ACADEMY OF AGRICULTURAL SCIENCES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The ricinole obtained by the traditional method is not high in purity, the crystallization process is troublesome, the preparation amount is small, and the loss is large

Method used

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  • Method for separating and preparing ricinine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Weigh 100 g of castor bean kernels, add 500 ml of petroleum ether and diethyl ether solution with a volume ratio of 2:1, extract with magnetic stirring at room temperature for 1 h, and filter with suction to obtain castor meal. Repeat the above steps 2 times, and the castor meal (filter cake) is air-dried.

[0028] Weigh 20 g of the filter cake, extract it with 200 ml of 95% (volume percent) ethanol aqueous solution for 3 h, concentrate the extract in vacuo at 45° C. to 20 ml, and freeze-dry in vacuo to obtain a crude extract of ricinine.

[0029] Using chloroform / methanol / water with a volume ratio of 2:1:1 as a two-phase solvent system, after mixing them thoroughly, let stand to separate the phases, and ultrasonically degas the two phases for 30 minutes respectively. Take the upper phase as the stationary phase and the lower phase as the mobile phase. Pump the stationary phase into a 325ml high-speed countercurrent chromatography separation column at a flow rate of 6m...

Embodiment 2

[0034] Weigh 100 g of castor bean kernels, add 800 ml of petroleum ether and diethyl ether solution with a volume ratio of 2:1, extract with magnetic stirring at room temperature for 2 h, and filter with suction. Repeat the above steps 3 times to air dry the filter cake.

[0035] Weigh 20g of filter cake, Soxhlet extraction with 160ml of 95% (volume percent) ethanol aqueous solution for 5h, the extract is concentrated in vacuo at 45°C to 15ml, and vacuum freeze-dried to obtain a crude extract of ricinine.

[0036] Use trichloromethane / methanol / water with a volume ratio of 5:4:2 as the two-phase solvent system, mix them thoroughly, and then let stand to separate the phases, and degas the two phases by ultrasonic wave for 30 minutes respectively. Take the upper phase as the stationary phase and the lower phase as the mobile phase. Pump the stationary phase into a 325ml high-speed countercurrent chromatography separation column at a flow rate of 6ml / min, start the high-speed cou...

Embodiment 3

[0038] The operation steps are the same as in Example 2, except that the mobile phase flow rate of high-speed countercurrent chromatography is 6ml / min, the volume ratio of the two-phase solvent system (chloroform / methanol / water) is 2:2:1, and the separation column speed is 500rpm, the volume The ratio of 2:1 petroleum ether and diethyl ether solution was 400ml, and 20g of the filter cake was extracted with 120ml of 95% (volume percent) ethanol aqueous solution for 5 hours by Soxhlet extraction. The yield of ricinine was 73%, and the purity was detected by HPLC according to the conditions of Example 1, reaching more than 98%.

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Abstract

The invention discloses a method for separating and preparing ricinine, which comprises the following steps: 1) extracting castor meal of castor seeds by extract to obtain crude extract of the ricinine; and 2) selecting a two-phase solvent system and adopting a high-speed counter current chromatography to separate and purify the crude extract of the ricinine obtained in step 1) to obtain the ricinine, wherein the two-phase solvent system in step 2) is methylene dichloride / methanol / water, or 1,2-dichloroethane / methanol / water, or methenyl chloride / methanol / water, and is preferably the methenyl chloride / methanol / water in the ratio of 2:1:1; the top phase in the two phases is an immobile phase, and the bottom phase is a mobile phase; and the rotating speed of a separation column for separation and purification is between 500 and 1,000 rpm, the flow rate of the mobile phase in the separation column is between 3 and 6ml / min, and the temperature of the two-phase solvent system in the separation column is between 20 and 30 DEG C. The ricinine prepared by the method has the purity of 98 percent.

Description

technical field [0001] The invention relates to a method for separating and preparing alkaloids, in particular to a method for separating and preparing ricinine. Background technique [0002] Ricinine is an alkaloid found in castor. Castor (Ricinus cammunis L) is a plant of the genus Castor in the Euphorbiaceae (Euphorbiaceae). It is one of the top ten oil crops in the world and is widely planted in the world. More than 90% of the world's total castor production. In my country, the main producing areas of castor are mainly Inner Mongolia, Jilin, Shandong and Shanxi. Castor beans contain about 50% castor oil, and castor meal after oil extraction contains about 35% protein. Castor meal contains ricinine, ricin, hemagglutinin, allergen toxoid, etc. Among them, ricinine and ricin have certain biological activities and have broad development and application prospects. As one of the toxic components in castor, ricinine has biological activities such as improving memory, protec...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D213/85A61P25/28A61P1/16A01P7/00A01P5/00
Inventor 石波梁平陈亚房苏晓鸥
Owner FEED RESEARCH INSTITUTE CHINESE ACADEMY OF AGRICULTURAL SCIENCES
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