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Method for separating and purifying a kind of chiral alkaloid rsmtca from Nitraria japonica seeds

A technology for the separation and purification of Nitraria japonica seeds, applied in the direction of organic chemistry, etc., to achieve the effects of good repeatability, convenient operation and simple process

Active Publication Date: 2017-03-01
CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There is no research report on the isolation and purification of rsMTCA from the seeds of Nitraria japonica

Method used

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  • Method for separating and purifying a kind of chiral alkaloid rsmtca from Nitraria japonica seeds
  • Method for separating and purifying a kind of chiral alkaloid rsmtca from Nitraria japonica seeds
  • Method for separating and purifying a kind of chiral alkaloid rsmtca from Nitraria japonica seeds

Examples

Experimental program
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Effect test

Embodiment 1

[0030] 1. Preparation of crude extract

[0031] After the Nitraria seeds are pulverized by a high-speed universal pulverizer, they are extracted in a traditional Chinese medicine decoction machine with a solid-liquid ratio of 1:10kg / L. The extraction time is 2h, and the extraction solvent is 75% ethanol, and the extraction times are 3 times. After three times of extraction, the extraction solutions were combined, the ethanol was recovered until there was no alcohol smell, and petroleum ether was added for repeated extraction. The aqueous layer extracted with petroleum ether was concentrated and evaporated to dryness on a rotary evaporator, dissolved in water, and preliminarily separated on D101 macroporous resin. The macroporous resin column is eluted, and the elution solution and concentration are: water, 10% V / V ethanol solution, and the 10% ethanol eluate is collected, concentrated and evaporated to dryness on a rotary evaporator for later use.

[0032] 2. Separation by hi...

Embodiment 2

[0037] 1. Preparation of crude extract

[0038] After the Nitraria seeds are pulverized by a high-speed universal pulverizer, they are extracted in a traditional Chinese medicine decoction machine with a solid-liquid ratio of 1:15kg / L for 3 hours, and the extraction solvent is 65% ethanol, and the number of extractions is 3 times. After three times of extraction, the extraction solutions were combined, the ethanol was recovered until there was no alcohol smell, and petroleum ether was added for repeated extraction. The aqueous layer extracted with petroleum ether was concentrated and evaporated to dryness on a rotary evaporator, dissolved in water, and preliminarily separated on D101 macroporous resin. The macroporous resin was eluted, and the elution solution and concentration were: water, 10% V / V ethanol solution, and the 10% ethanol eluate was collected, concentrated and evaporated to dryness on a rotary evaporator for later use.

[0039] 2. Separation by high-speed counte...

Embodiment 3

[0044] 1. Preparation of crude extract

[0045] After the Nitraria seeds are pulverized by a high-speed universal pulverizer, they are extracted in a traditional Chinese medicine decoction machine with a solid-liquid ratio of 1:8kg / L for 1.5 hours, and the extraction solvent is 95% ethanol, and the number of extractions is 3 times. After three times of extraction, the extraction solutions were combined, the ethanol was recovered until there was no alcohol smell, and petroleum ether was added for repeated extraction. The aqueous layer extracted with petroleum ether was concentrated and evaporated to dryness on a rotary evaporator, dissolved in water, and preliminarily separated on D101 macroporous resin. The macroporous resin was eluted, and the elution solution and concentration were: water, 10% V / V ethanol solution, and the 10% ethanol eluate was collected, concentrated and evaporated to dryness on a rotary evaporator for later use.

[0046] 2. Separation by high-speed count...

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Abstract

The present invention provides a method for separating and purifying (1R, 3S)-1-methyl-1,2,3,4-tetrahydro-beta-carboline-3-carboxylic acid(rsMTCA) from nitraria seeds. According to the present invention, highly pure rsMTCA is obtained from nitraria by using a high-speed countercurrent chromatography and using an appropriate solvent system, and the technique can quickly, high efficiently separate and prepare (1R, 3S)-1-methyl-1,2,3,4-tetrahydro-beta-carboline-3-carboxylic acid (rsMTCA) with low costs and no pollution without using a solid phase support, and there is no irreversible adsorption, and no loss is incurred to samples. The present invention is simple in process, convenient in operation, safe and good in repeatability, and can applied to industrial production.

Description

technical field [0001] The invention relates to a method for separating and purifying a chiral alkaloid from Nitraria japonica seeds. Background technique [0002] The seeds of Nitraria thorn contain a variety of active ingredients. At present, many active substances have been isolated from the seeds of Nitraria thorn, mainly including the following types of substances, flavonoids: quercetin, isorhamnetin-7-O-α-L- Rhamnoside, Kaempferin-7-O-α-L-Rhamnoside, Isorhamnetin-7-O-β-D-Glucoside, Quercetin-7-O-α-L-Rhamnoside Liglucoside, isorhamnose, allantoin, carotin, isorhamnose; alkaloids: L-tryptophan, allantoin and 1-methyl-1,2,3,4-tetrahydro -β-carboline-3-carboxylic acid (1-Methyl-1,2,3,4-tetrahydro-β-carboline-3-carboxylic acid, MTCA for short). [0003] MTCA belongs to the indole alkaloids, the current research on indole alkaloids has become a hot spot of anti-tumor drugs, especially in the discovery of new drugs and new drug lead compounds play an irreplaceable role. Th...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D471/04
CPCC07D471/04
Inventor 胡娜索有瑞周武韩丽娟
Owner CHINA ACAD OF SCI NORTHWEST HIGHLAND BIOLOGY INST