Extraction and preparation method of abamectin B2a

Abstract

The invention discloses an extraction and preparation method of abamectin B2a, which comprises the following steps: preparing an abamectin fermentation liquid into dry mycelia, and leaching; concentrating the leaching liquor, and adding toluene and other extractants to carry out extraction; crystallizing the extract I; concentrating the mother solution into ointment; adding toluene into the ointment to obtain an extract II; adding a filter aid into the extract II, stirring, cooling, crystallizing, growing the grain, and carrying out vacuum filtration; adding toluene to dissolve the filter cake, heating the filtrate, cooling, crystallizing, growing the grain, and carrying out vacuum filtration to obtain an abamectin B2a crystal crude product; and recrystallizing the abamectin B2a crystal crude product to obtain the abamectin B2a crystal fine product. The method disclosed by the invention can effectively separate the abamectin B2a from the abamectin fermentation liquid, and has the advantages of high extraction rate and favorable purification effect.

Description

technical field

[0001] The invention relates to an extraction and preparation method of antibiotics, in particular to an extraction and preparation method of avermectin B2a. Background technique

[0002] Abamectin is a new type of antibiotic pesticide developed in my country in the past 20 years. It is a microbial fermentation product and is currently the most ideal pesticide product to replace highly toxic organophosphorus pesticides. Abamectin is a group of 16-membered macrolide antibiotics with similar structure isolated and extracted from the fermentation product of Streptomyces avermitilis in Streptomyces. It consists of a group of 8 homologues with similar structures, B1 and B2 are two major classes of components in this homologue. 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. Component B1 has the highest t...

Examples

Embodiment 1

[0034] Refer to the process figure 1 , the specific steps are:

[0035] a, using the abamectin fermented liquid as the starting material, pumping it into the plate frame for filtration. In order to increase the filtration rate, an appropriate amount of filter aid can be added to the abamectin fermentation broth, and the fermentation broth can also be heated to 80°C to 90°C. Mycelium is obtained after filtering, and then dried to obtain dry mycelium. Place the dried mycelium in a reaction tank, add ethanol to soak and extract (referred to as extraction). The add-on of ethanol is advisable with being able to immerse mycelium completely, and the concentration of ethanol can be selected according to the range shown with conventional leaching method, and the present invention is preferably with 75-95%. After the dried mycelium is soaked in ethanol for 2-5 hours, the extract is collected and set aside; the filter residue can be repeatedly extracted with ethanol for 2-3 times, and...

Embodiment 2

[0049] Refer to the process figure 1 , the specific steps are:

[0050] a, using the abamectin fermented liquid as the starting material, pumping it into the plate frame for filtration. Mycelium is obtained after filtering, and then dried to obtain dry mycelium. The mycelium is placed in a reaction tank, and 85% ethanol is added for extraction. The addition of ethanol is advisable to be able to submerge mycelium completely. After the mycelium was soaked in ethanol for 3 hours, the extract was collected for subsequent use;

[0051] b. Pour the extract into the evaporating tank, heat to concentrate the extract until it does not contain ethanol, then add a certain amount of toluene and water, heat up to 80-100°C, stir for 30min-40min, let stand, and discharge to the bottom aqueous solution, and the organic solution was collected to obtain the extract I.

[0052] c. Add perlite filter aid to the extract Ⅰ, stir for 30-40 minutes, and after stirring evenly, cool down to 10-0°C...

Embodiment 3

[0055] a, using the abamectin fermented liquid as the starting material, pumping it into the plate frame for filtration. Mycelium is obtained after filtering, and then dried to obtain dry mycelium. Place the mycelium in a reaction tank, add 60% ethanol for extraction. The addition of ethanol is advisable to be able to submerge mycelium completely. After the mycelium is soaked in ethanol for 5-6 hours, the extract is collected and set aside;

[0056] b. Pour the extract solution into the evaporating tank, heat and concentrate the extract solution to contain no ethanol, then equal amount of DMF, stir for 20min~30min, let it stand still, discharge the aqueous solution at the bottom, collect the organic solution, and obtain the extract solution Ⅰ .

[0057] c. After removing DMF from the extract solution I, add 1% diatomaceous earth filter aid to the obtained material solution, stir for 20-30 minutes, after stirring evenly, cool down to 5-0°C for crystallization, after a large ...

technical field

[0001] The invention relates to an extraction and preparation method of antibiotics, in particular to an extraction and preparation method of avermectin B2a. Background technique

[0002] Abamectin is a new type of antibiotic pesticide developed in my country in the past 20 years. It is a microbial fermentation product and is currently the most ideal pesticide product to replace highly toxic organophosphorus pesticides. Abamectin is a group of 16-membered macrolide antibiotics with similar structure isolated and extracted from the fermentation product of Streptomyces avermitilis in Streptomyces. It consists of a group of 8 homologues with similar structures, B1 and B2 are two major classes of components in this homologue. 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. Component B1 has the highest t...

Examples

Embodiment 1

[0034] Refer to the process figure 1 , the specific steps are:

[0035] a, using the abamectin fermented liquid as the starting material, pumping it into the plate frame for filtration. In order to increase the filtration rate, an appropriate amount of filter aid can be added to the abamectin fermentation broth, and the fermentation broth can also be heated to 80°C to 90°C. Mycelium is obtained after filtering, and then dried to obtain dry mycelium. Place the dried mycelium in a reaction tank, add ethanol to soak and extract (referred to as extraction). The add-on of ethanol is advisable with being able to immerse mycelium completely, and the concentration of ethanol can be selected according to the range shown with conventional leaching method, and the present invention is preferably with 75-95%. After the dried mycelium is soaked in ethanol for 2-5 hours, the extract is collected and set aside; the filter residue can be repeatedly extracted with ethanol for 2-3 times, and...

Embodiment 2

[0049] Refer to the process figure 1 , the specific steps are:

[0050] a, using the abamectin fermented liquid as the starting material, pumping it into the plate frame for filtration. Mycelium is obtained after filtering, and then dried to obtain dry mycelium. The mycelium is placed in a reaction tank, and 85% ethanol is added for extraction. The addition of ethanol is advisable to be able to submerge mycelium completely. After the mycelium was soaked in ethanol for 3 hours, the extract was collected for subsequent use;

[0051] b. Pour the extract into the evaporating tank, heat to concentrate the extract until it does not contain ethanol, then add a certain amount of toluene and water, heat up to 80-100°C, stir for 30min-40min, let stand, and discharge to the bottom aqueous solution, and the organic solution was collected to obtain the extract I.

[0052] c. Add perlite filter aid to the extract Ⅰ, stir for 30-40 minutes, and after stirring evenly, cool down to 10-0°C...

Embodiment 3

[0055] a, using the abamectin fermented liquid as the starting material, pumping it into the plate frame for filtration. Mycelium is obtained after filtering, and then dried to obtain dry mycelium. Place the mycelium in a reaction tank, add 60% ethanol for extraction. The addition of ethanol is advisable to be able to submerge mycelium completely. After the mycelium is soaked in ethanol for 5-6 hours, the extract is collected and set aside;

[0056] b. Pour the extract solution into the evaporating tank, heat and concentrate the extract solution to contain no ethanol, then equal amount of DMF, stir for 20min~30min, let it stand still, discharge the aqueous solution at the bottom, collect the organic solution, and obtain the extract solution Ⅰ .

[0057] c. After removing DMF from the extract solution I, add 1% diatomaceous earth filter aid to the obtained material solution, stir for 20-30 minutes, after stirring evenly, cool down to 5-0°C for crystallization, after a large ...

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