Extraction method for improving output and internal quality of avermectin B1a fine powder

A technology of abamectin and quality, applied in the field of pesticide preparation, can solve the problems of large amount of methanol used, low extraction titer, low content of abamectin B1a, etc., achieves reduction of recrystallization times, overcomes low yield, The effect of quality improvement

Active Publication Date: 2017-02-08
QILU PHARMA INNER MONGOLIA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0009] Aiming at the low extraction potency and large amount of methanol used in the existing abamectin extraction process; the technical problems of low abamectin B1a content and poor intrinsic quality caused by many oils and esters in the refined powder, a method of improving the abamectin content of the present invention Extraction method of B1a fine powder production capacity and intrinsic quality

Method used

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  • Extraction method for improving output and internal quality of avermectin B1a fine powder
  • Extraction method for improving output and internal quality of avermectin B1a fine powder
  • Extraction method for improving output and internal quality of avermectin B1a fine powder

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] A kind of extraction method that improves production capacity and internal quality of Abamectin B1a fine powder, comprises steps as follows:

[0041] (1) Take 2000g of dried mycelium of abamectin (mycelia potency is 10230μ / g), add 10000mL of methanol with a temperature of 40°C and a mass concentration of 95%, stir for 30 minutes, and filter to obtain the abamectin extraction Liquid 9900ml, with HPLC, the resulting extract is detected, and the potency of the extract is 20842μ / ml.

[0042] (2) Take 5 L of the extract and freeze it at 0°C for 4 hours. After the flocs are precipitated, the filtrate is obtained by suction filtration.

[0043] (3) The filtrate of step (2) is heated up to 65° C., concentrated under vacuum conditions to obtain a thick ointment, and 80° C. of hot water is added to the thick ointment. The amount of hot water is the same as that of the thick ointment The volume ratio of the mixture is 1:2, stirred for 30 minutes, then allowed to stand for 15 minu...

Embodiment 2

[0058] A kind of extraction method that improves production capacity and internal quality of Abamectin B1a fine powder, comprises steps as follows:

[0059] (1) Take 2000g of dried mycelium of abamectin (mycelia potency is 10230μ / g), add 10000mL of methanol with a temperature of 42°C and a mass concentration of 96%, stir for 30 minutes, and filter to obtain the abamectin extraction Liquid 9900ml, with HPLC, the obtained extract is detected, and the potency of the extract is 20143μ / ml.

[0060] (2) Take 5L of the extract and freeze it at 0°C for 3 hours. After the flocs are precipitated, the filtrate is obtained by suction filtration. The filtrate is kept at 0°C to keep warm, and no flocs are precipitated.

[0061] (3) The filtrate of step (2) is heated up to 70°C, concentrated under vacuum to obtain a thick ointment, and 78°C of hot water is added to the thick ointment, the amount of hot water is the same as that of the thick ointment The volume ratio is 1:3, stir for 30 minu...

Embodiment 3

[0076] A kind of extraction method that improves production capacity and internal quality of Abamectin B1a fine powder, comprises steps as follows:

[0077] (1) Take 2000g of dried mycelium of abamectin (the potency of mycelia is 10230μ / g), add 10000mL of methanol with a temperature of 45°C and a mass concentration of 96%, stir for 30 minutes, and filter to obtain the abamectin extraction Liquid 9900ml, with HPLC, the obtained extract is detected, and the potency of the extract is 20617μ / ml.

[0078] (2) Take 5 L of the extract and freeze it at -1°C for 2 hours. After the flocs are precipitated, the filtrate is obtained by suction filtration. The filtrate is kept at 0°C to keep warm, and no flocs precipitate.

[0079] (3) The filtrate of step (2) is heated up to 68°C, concentrated under vacuum conditions to obtain a thick ointment, and 82°C of hot water is added to the thick ointment, the amount of hot water is the same as that of the thick ointment The volume ratio of the mi...

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Abstract

The invention relates to an extraction method for improving the output and internal quality of avermectin B1a fine powder. The method comprises the following steps: adding hyphae of avermectin into a methanol solvent with a temperature of 40 to 45 DEG C and a mass concentration of 95 to 97%, carrying out extraction, then cooling to a temperature lower than 0 DEG C, maintaining the temperature for 2 to 4 hours, concentrating and purifying filtrate, and finally carrying out crystallization and recrystallization to obtain the avermectin B1a crystals. The hyphae of avermectin is added into methanol with a temperature of 40 to 45 DEG C and a mass concentration of 95 to 97% to obtain an extract; as the extract cools down, the solubility of higher fatty acid grease in the methanol is reduced quickly, the higher fatty acid grease is precipitated, after filtering, the crystallization and recrystallization will remove grease residues from the fine powder, thus the content of avermectin B1a is increased, and the internal quality of fine powder is improved therefore.

Description

[0001] Technical field: [0002] The invention relates to a preparation method of biological pesticides, in particular to an extraction method for improving the production capacity and internal quality of abamectin B1a fine powder, and belongs to the technical field of pesticide preparation. [0003] Background technique: [0004] 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 biological insecticidal activity against nematodes, insects and mites. [0005] Abamectin is currently one of the most effective pesticides in the world, with an annual domestic usage of about 4,100 tons, making it a leading product among pesticides and insecticides. Abamectin is the most broad-spectrum, efficient, safe and stable insecticide. It has a strong activity of killing mites, insects and parasites. It can also be used for huma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07H17/08C07H1/06
CPCC07H1/06C07H17/08
Inventor 梁振兵刘世宽安文俊程宏
Owner QILU PHARMA INNER MONGOLIA
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