Method for extracting residual abamectin

A technology of abamectin and oily liquid, which is applied in the field of separation and extraction of effective component B1 and related biologically active components, can solve the problems of failure to achieve success, difficulty in extracting active components of abamectin crystallization mother liquor, etc., and achieve Low cost, cheap solvent, and high crystallization yield

Active Publication Date: 2010-09-22
浙江拜克生物科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The purpose of the present invention is to provide a method for extracting residual abamectin for the problem that the active components of the current abamectin crystallization mother liquor are difficult to extract. It uses column chromatography under appropriate temp

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

Example one:

(1) Take 14 kg of abamectin crystallization mother liquor and remove the solvent at 70°C and a vacuum of 0.08 MPa to obtain 10 kg of the first oily liquid. Analyzed by HPLC, the oily liquid contained B1a5.5%, B2a16.7%, A2a14.2%, and A1a11.1%;

(2) Add 10 liters of ethyl acetate and 5 liters of petroleum ether as mobile phase to the first oily liquid, and reflux and dissolve at 60°C for later use;

(3) After the silica gel column is eluted with the mobile phase to equilibrate, the liquid level is lowered to a decent bed level for use;

(4) Load the sample, slowly add the first oily liquid dissolved in the mobile phase to the surface of the chromatography column bed, then pressurize and open the lower eluent outlet to make the sample liquid completely enter the bed, Close the lower eluent outlet, slowly fill the bed with mobile phase, and seal it with the storage tank that stores the mobile phase; open the lower outlet, and gradually increase the pressure to 0.5Mpa af...

Example Embodiment

Step C2:

(1) Take 14 kg of abamectin crystallization mother liquor and remove the solvent at 70°C and a vacuum of 0.08 MPa to obtain 10 kg of the first oily liquid. Analyzed by HPLC, the oily liquid contained B1a5.5%, B2a16.7%, A2a14.2%, and A1a11.1%;

(2) Add 14 liters of ethyl acetate and 7 liters of petroleum ether as mobile phase to the first oily liquid, reflux and dissolve at 50°C for use;

(3) After the silica gel column is eluted with the mobile phase to equilibrate, the liquid level is lowered to a decent bed level for use;

(4) Load the sample, slowly add the first oily liquid dissolved in the mobile phase to the surface of the chromatography column bed, then pressurize and open the lower eluent outlet to make the sample liquid completely enter the bed, Close the eluent outlet at the bottom, slowly fill the bed with mobile phase, and seal it with the storage tank that stores the mobile phase; open the lower outlet, and gradually increase the pressure to 1.5MPa after el...

Example Embodiment

Example three:

(1) Take the oily substance containing the four components A1a, A2a, B1b, B1a, and B2a obtained in step (4) of Example 1, and dissolve it with ethyl acetate / methanol with a volume ratio of 2 / 1 to obtain a sample solution ;

(2) After the silica gel column is equilibrated with the mobile phase, add the above sample solution to the surface of the balanced silica gel column bed, then open the lower outlet, wait for the sample solution to completely enter the column bed and start elution with the mobile phase. The temperature is 60℃, the column pressure is 3MPa, the mobile phase is ethyl acetate / chloroform / dichloromethane / methanol with a volume ratio of 9 / 9 / 2 / 1; online detection with UV detector, the first component that flows out is Component A (A1a+A2a), then component B (B1a+B2a), were recovered separately, the eluent containing component B was distilled under reduced pressure to remove the solvent, and then ethanol was added to reflux and dissolve at 70°C, and th...

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PUM

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Abstract

The invention relates to a method for extracting residual abamectin from crystallization mother liquor, which comprises the steps of removing ester impurities and further separating each component by using a C18 column or a silica gel column. The separation and extraction process is simple; the selected and used solvent is cheap, safe and environment-friendly, and meets the industrialized requirement; and the effective ingredient B1 has high yield and reaches about 90 percent.

Description

technical field [0001] The present invention relates to a method for extracting residual biologically active antibiotic components from antibiotic waste liquid, in particular to a method for separating and extracting effective component B1 and related biologically active components from the crystallization mother liquor of abamectin method. Background technique Abamectin, the English name Avermectins, is a class of sixteen-membered macrolide compounds with insecticidal, acaricidal and nematicidal activities first developed by Satoshi Omura of Kitasato University in Japan and Merck Company of the United States. Abamectin has been widely used in the prevention and control of animal parasitic diseases and crop pests since it came out in the early 1980s. Avermectin consists of 8 components: A1a, A1b, A2a, A2b, B1a, B1b, B2a, and B2b. There are mainly 4 types, namely A1a, A2a, B1a, and B2a, among which avermectin B1a has the strongest biological activity. The production proc...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/08
Inventor 沈德堂储消和潘贞德吴雪萍
Owner 浙江拜克生物科技有限公司
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