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Preparation method of high-purity abamectin B2a

A high-purity technology of abamectin, applied in the field of biopesticide preparation, can solve the problems of on-site personnel's danger, low crystal purity, high production cost, etc., and achieve the goal of reducing production cost, high crystal purity, and less crystallization times Effect

Active Publication Date: 2015-05-27
QILU PHARMA INNER MONGOLIA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this method provides a relatively low production cost and is easy to industrialize the extraction and preparation of Abamectin B2a, the method uses the carcinogen toluene as the crystallization and recrystallization solvent, which causes physical harm to the on-site employees during the production operation. Harmful and pollute the environment
In addition, the purity of B2a crystals obtained by this process through two recrystallizations is relatively low, with a purity of only 90%.
[0004] Chinese patent document CN103333214A discloses a kind of preparation method of abamectin B2a refined powder, adopts 0.25-0.6% tetrabutylammonium bromide aqueous solution to wash sec-butyl acetate extract, makes avermectin purity improve to In this patent, although the purity of abamectin has been improved to a certain extent, the process uses carcinogenic aromatic hydrocarbons as crystallization and recrystallization solvents, which is dangerous to on-site personnel during production operations, and In the process, sec-butyl acetate is firstly used for extraction, and after washing with water, the sec-butyl acetate is vacuum distilled and then crystallized with aromatic hydrocarbons. The process is more complicated and the production cost is higher.

Method used

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  • Preparation method of high-purity abamectin B2a

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]A preparation method for high-purity Abamectin B2a, comprising steps as follows:

[0038] 1. Take 1500ml of abamectin B1a crystallization mother liquor after crystallization and separation of abamectin B1a in the production process of abamectin B1a and raise the temperature to 70°C, keep the temperature and distill most of the distillate under vacuum until the ointment is obtained For thick materials, the vacuum degree under vacuum conditions is 0.06Mpa;

[0039] 2. Take 450g of the ointment thick material obtained in step 1, add 1125ml of n-butyl acetate, heat up to 70°C, stir for 0.5 hours until the ointment thick material is completely dissolved, and obtain an extract, add 350ml of saturated saline, and stir at 80°C 2 hours, then stand for 15 minutes to separate layers, remove the water phase, and repeat washing twice to obtain n-butyl acetate solution;

[0040] 3. First cool the n-butyl acetate solution to 20°C quickly with a water bath, then adjust the stirring spe...

Embodiment 2

[0043] A preparation method for high-purity Abamectin B2a, comprising steps as follows:

[0044] 1. Take 1500ml of the abamectin B1a crystallization mother liquor after crystallization and separation of abamectin B1a during the production process of abamectin B1a and heat up to 80°C, keep the temperature and distill for 2h under a vacuum condition of 0.065Mpa, distill Most of the distillate is removed until the ointment thick material is obtained,

[0045] 2. Take 440g of the ointment thick material obtained in step 1, add 1100ml of n-butyl acetate, heat up to 60°C, stir for 1 hour until the ointment thick material is completely dissolved, and obtain an extract, add 430ml of saturated saline, and stir at 85°C 1 hour, and then stand for 15 minutes to separate layers, remove the water phase, and repeat washing twice to obtain n-butyl acetate solution;

[0046] 3. First, quickly cool the n-butyl acetate solution to 20°C with a water bath, then adjust the stirring speed to 10r / mi...

experiment example

[0055] Adopt area normalization method to test the purity of embodiment 1 and comparative example 1 Abamectin B2a refined powder,

[0056] Powder detection method: high performance liquid chromatography area normalization method

[0057] Instrument: high performance liquid chromatography

[0058] Chromatographic conditions: mobile phase (methanol: water = 85:15)

[0059] Detection and wavelength: UV, 245nm

[0060] Chromatographic column (C18, 4.6mm*250mm)

[0061] Flow rate: 1ml / min

[0062] Injection volume: 20ul

[0063] Test steps: Weigh 0.025-0.030g of fine powder into a 100ml volumetric flask, dissolve with methanol, and make to volume. Draw 20ml of the solution and inject it into the high-efficiency chromatograph. According to the above chromatographic conditions, the detection time is 15 minutes, and the peak time of B2a is about 5 minutes. The purity of B2a is calculated according to the area normalization method. The purity of the Abamectin B2a fine powder of t...

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Abstract

The invention relates to a preparation method of high-purity abamectin B2a, which comprises the following steps: concentrating an abamectin B1a crystal mother solution to no fraction under vacuum conditions, thereby obtaining an ointment thick material; adding an extractant, extracting to obtain an extract, washing the extract with a saturated saline solution 2-3 times, and removing the water phase to obtain an n-butyl acetate solution; cooling the obtained n-butyl acetate solution to crystallize, growing the grain, and carrying out vacuum filtration to obtain an abamectin B2a coarse crystal; and recrystallizing the abamectin B2a coarse crystal, carrying out vacuum filtration, and drying to obtain the high-purity abamectin B2a refined powder. The environment-friendly nontoxic solvent n-butyl acetate is used instead of the toxic solvent aromatic hydrocarbon to produce the abamectin B2a refined product, so the harm to the in-field personnel body is low in the production operation process, and the environmental pollution is small. By using the n-butyl acetate as the crystallizing solvent of the B2a, the purity of the abamectin B2a refined powder is higher than 95%.

Description

Technical field: [0001] The invention relates to a preparation method of biological pesticides, in particular to a preparation method for extracting high-purity avermectin B2a by using an environment-friendly crystallization solvent, and belongs to the technical field of pesticide preparation. Background technique: [0002] Abamectin is a group of 16-membered macrolide antibiotics with similar structure isolated and extracted from the fermentation product of Streptomyces. of the two components. Abamectin B components have extremely high bioinsecticidal activity against nematodes, insects, and mites, but there are significant differences in the insecticidal abilities B1a and B2a of different targets. Abamectin B2a has a good effect on root-knot nematodes. According to reports such as Putter in 1981, in the 8 components of abamectin, B1a and B2a are the most effective agricultural active substances, and wherein B2a has the effect on plant root-knot nematodes. Nematodes are t...

Claims

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Application Information

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IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 梁振兵刘世宽安文俊
Owner QILU PHARMA INNER MONGOLIA
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