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Method for extracting purified rape antitoxin

An antitoxin and brassica technology, which is applied in organic chemistry, bulk chemical production, etc., can solve the problems that there are no research reports on the extraction of brassica antitoxin, and there are few researches on the chemical components of mustard, and achieve stable process, high purity and low operating temperature Effect

Inactive Publication Date: 2012-09-19
NANJING ZELANG MEDICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] At present, there are few studies on the chemical constituents of mustard, and there is no report on the extraction of Brassica antitoxin

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Crush the mustard leaves, pass through a 20-mesh sieve, weigh 10kg and add it to the extraction kettle, turn on the machine, and adjust the parameters: the extraction temperature is 35°C, the extraction pressure is 28MPa, the temperature of the separation kettle I is 25°C, the pressure is 18MPa, and the separation kettle II The temperature is 20°C, the pressure is 8MPa, and CO is fed at a flow rate of 40L / h 2 Extract for 2 hours, analyze the extract, adjust the pH to 9 with ammonia water, add dichloromethane to extract several times, collect and combine the dichloromethane extracts, concentrate under reduced pressure and add alumina medium pressure column (400 mesh neutral alumina, The ratio of column diameter to height is 1:5), followed by elution according to the volume ratio of dichloromethane-methanol 20:1, 10:1, 5:1, 5:2, TLC tracking detection, collecting high-concentration fractions, and recovering reagents , and dried to obtain 408mg of brassica antitoxin produc...

Embodiment 2

[0017] Crush the mustard leaves, pass through a 20-mesh sieve, weigh 10kg and add it to the extraction kettle, turn on the machine, and adjust the parameters: the extraction temperature is 55°C, the extraction pressure is 20MPa, the temperature of the separation kettle I is 45°C, the pressure is 10MPa, and the separation kettle II The temperature is 35°C, the pressure is 8MPa, and CO is fed at a flow rate of 40L / h 2 Extract for 4 hours, analyze the extract, adjust the pH to 9 with ammonia water, then add dichloromethane to extract several times, collect and combine the dichloromethane extracts, concentrate under reduced pressure and add alumina medium pressure column (200 mesh neutral alumina, The ratio of column diameter to height is 1:7), followed by elution according to the volume ratio of dichloromethane-methanol 20:1, 10:1, 5:1, 5:2, TLC tracking detection, collecting high-concentration fractions, and recovering reagents , and dried to obtain 375 mg of brassica antitoxin ...

Embodiment 3

[0019] Crush the mustard leaves, pass through a 20-mesh sieve, weigh 10kg and add it to the extraction kettle, turn on the machine, and adjust the parameters: the extraction temperature is 45°C, the extraction pressure is 25MPa, the temperature of the separation kettle I is 28°C, the pressure is 15MPa, the separation kettle II The temperature is 25°C, the pressure is 6MPa, and CO is fed at a flow rate of 40L / h 2 Extract for 3 hours, analyze the extract, adjust the pH to 9 with ammonia water, then add dichloromethane to extract several times, collect and combine the dichloromethane extracts, concentrate under reduced pressure and add alumina medium pressure column (300 mesh neutral alumina, The ratio of column diameter to height is 1:7), followed by elution according to the volume ratio of dichloromethane-methanol 20:1, 10:1, 5:1, 5:2, TLC tracking detection, collecting high-concentration fractions, and recovering reagents , and dried to obtain 345 mg of brassica antitoxin prod...

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PUM

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Abstract

The invention discloses a method for extracting purified rape antitoxin. The method is characterized in that mustard leaves are used as raw materials, CO2 is used as the solvent for supercritical extraction for 2-4 hours, the pH of analytical objects is adjusted to be 9 by aid of ammonia water, dichloromethane is added for extracting, an alumina medium-pressure column is added into dichloromethane extract liquor, the liquor rinsed to be neutral, dichloromethane-methanol mixed solution is used for eluting, the thin-layer chromatography (TLC) is used for tracking and detecting, high-concentration current is collected, the solvent is recycled, and rape antitoxin is obtained after drying. The method is simple in process, small in pollution, high in yield and high in product purity.

Description

technical field [0001] The invention belongs to the field of extraction and separation of effective plant components, and in particular relates to a method for extracting and purifying brassica antitoxin. Background technique [0002] Brassilexine is a white crystal, an indole alkaloid with the molecular formula C 9 h 6 N 2 S, molecular weight 174.23, derived from Cruciferae mustard Brassica juncea L.'s leaf. Pharmacological studies have shown that Brassica antitoxin has anti-tumor effect, inhibits the growth of human cancer cells, and its LD50 is 8 μg / mL. At a concentration of 20 μg / mL, it has cytotoxic activity and can inhibit KB cells by 100%. In addition, Brassica antitoxin has antifungal activity in vitro. [0003] Mustard greens, (scientific name: Brassica juncea L), is an annual or biennial herb of the genus Brassica. Also known as potherb mustard. It has the effects of clearing the lungs and expelling phlegm, warming the middle and promoting Qi. It is mai...

Claims

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Application Information

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IPC IPC(8): C07D513/04
CPCY02P20/54
Inventor 刘东锋杨成东
Owner NANJING ZELANG MEDICAL TECH
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