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 difficult extraction of active components of abamectin crystallization mother liquor, and achieve cheap solvents and easy operation Simple, simple separation and extraction process

Active Publication Date: 2012-03-14
浙江拜克生物科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] 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 temperature and pressure control to make the effective components The crystallization yield is more than 90%, which meets the needs of the industrial sector and solves the technical problems that people have been eager to solve for a long time but have not been successful.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] (1) Get 14 kg of abamectin crystallization mother liquor, and remove the solvent under the condition of 0.08 MPa at 70 DEG C and a vacuum degree to obtain 10 kg of the first oily liquid. After HPLC analysis by high performance liquid chromatography, the oily liquid contained B1a 5.5%, B2a 16.7%, A2a 14.2%, A1a 11.1%;

[0034] (2) Add 10 liters of ethyl acetate and 5 liters of sherwood oil into the first oily liquid as mobile phase, refluxing and dissolving at 60°C for subsequent use;

[0035] (3) After the silica gel column is eluted with mobile phase and balanced, the liquid level is reduced to the bed level for subsequent use;

[0036] (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 outflow port, so that the sample liquid completely enters the bed, Close the eluent outlet at the lower part, slowly fill up the mobile phase above the bed body, ...

Embodiment 2

[0039] (1) Get 14 kg of abamectin crystallization mother liquor, and remove the solvent under the condition of 0.08 MPa at 70 DEG C and a vacuum degree to obtain 10 kg of the first oily liquid. After HPLC analysis by high performance liquid chromatography, the oily liquid contained B1a 5.5%, B2a 16.7%, A2a 14.2%, A1a 11.1%;

[0040] (2) Add 14 liters of ethyl acetate and 7 liters of sherwood oil into the first oily liquid as mobile phase, refluxing and dissolving at 50°C for subsequent use;

[0041] (3) After the silica gel column is eluted with mobile phase and balanced, the liquid level is reduced to the bed level for subsequent use;

[0042] (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 outflow port, so that the sample liquid completely enters the bed, Close the lower eluent outflow port, slowly fill up the mobile phase above the bed body, and se...

Embodiment 3

[0045] (1) Get the oily matter containing A1, A2, B1 and B2 four components obtained in step (4) of Example 1, and dissolve it in ethyl acetate / methanol with a volume ratio of 2 / 1 to obtain a sample solution;

[0046] (2) After the silica gel column is equilibrated with the mobile phase, the above-mentioned sample solution is added to the surface of the well-balanced silica gel column bed, and then the lower outlet is opened. After the sample solution has completely entered the column bed, the mobile phase begins to elute. The temperature is 60°C, the column pressure is 3MPa, and the mobile phase is ethyl acetate / chloroform / dichloromethane / methanol with a volume ratio of 9 / 9 / 2 / 1; it is detected online with an ultraviolet detector, and the component that flows out first is Component A (A1a+A2a+A1b+A2b), followed by component B (B1a+B2a+B1b+B2b), were recovered separately, and the eluent containing component B was distilled off under reduced pressure to remove the solvent, and th...

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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 [0002] 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. [0003] 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. [0...

Claims

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Application Information

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Patent Type & Authority Patents(China)
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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