A kind of preparation method of Abamectin

A technology of abamectin and purpose, applied in the field of high-purity abamectin, can solve the problems of small batch volume, pollute the environment, high cost, etc., and achieve the effects of controllable quality, stable yield and low cost

Active Publication Date: 2015-10-28
NORTH CHINA PHARMA GROUP AINO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a kind of technique simple, stable yield, the preparation technique of the high-purity abamectin B1 that can scale production component ratio controllable, to solve the step loaded down with trivial details that existing separation and purification method exists, Small batch volume, high cost and environmental pollution

Method used

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  • A kind of preparation method of Abamectin
  • A kind of preparation method of Abamectin
  • A kind of preparation method of Abamectin

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Embodiment 1: the preparation of Abamectin crude product:

[0026] The components of slant culture medium, seed culture medium and fermentation medium used in this embodiment are as follows:

[0027] Slant medium: 15g glucose, 3g beef extract, 0.5g asparagine, 0.5g KH2PO4, 19g agar, add tap water to dissolve and adjust the volume to 1000ml, adjust the pH value to 7.2~7.5; sterilize at 121°C for 30min.

[0028] Seed medium: 30.0g cornstarch, 8.0g soybean powder, 10g peanut cake powder, 5.0g yeast powder, 2.0g COCl2, add tap water to dissolve, dilute to 1000 ml, pH value 6.8-6.9, sterilize at 121 ℃ 30 min.

[0029] Fermentation medium: 150.0g corn starch, 30.0g soybean powder, 9.0g yeast powder, (NH4)2SO4 0.25g, COCl2 0.03g, Na2MoO4 0.025g, MnSO4 0.003g, CaCO3 1.0g, amylase 0.03g, add tap water Dissolve and dilute to 1000 ml, pH 7.2-7.4, and sterilize at 121°C for 30 minutes.

[0030] (1) Inoculate the strain of Streptomyces averditilis (No. 192S9) on the slant medium,...

Embodiment 2

[0032] Embodiment 2: Abamectin crude product purification treatment

[0033]Get the Abamectin crude product 5g that embodiment 1 prepares, dissolve with 20mL acetone, load the chromatographic column (loading capacity is 500ml) to ODS reverse-phase chromatographic filler, at first use the ethanol aqueous solution (volume concentration 60%) of 10L as Mobile phase elution, and then use 75% ethanol aqueous solution as mobile phase elution (flow rate is 2BV / h), until all abamectins flow out, liquid phase detection 75% ethanol eluent, combined elution according to the detection results Deliquification, concentration, and vacuum drying at 45°C yielded 1.5 g of abamectin B1 (B1a+B1b) with a purity of 99.0% (see Tables 1 and 2 for the proportions of each component).

Embodiment 3

[0034] Embodiment 3: Abamectin crude product purification process

[0035] Get the Abamectin crude product 10g that embodiment 1 prepares, dissolve with 50mL acetone, load the chromatographic column (loading capacity is 1000ml) to ODS reverse-phase chromatographic filler, at first use the methanol aqueous solution (volume concentration 70%) of 15L as Elute with mobile phase, then elute with 85% methanol aqueous solution (flow rate: 4BV / h), until all the abamectin flows out, detect the 85% methanol eluate in liquid phase, combine the eluate according to the detection results, Concentrated and dried under vacuum at 45 °C to obtain 4.1 g of Abamectin B1 (B1a+B1b) with a purity of 99.4% (see figure 2 , The proportion of each component is shown in Table 1 and 2).

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Abstract

The invention discloses a method for preparing high-purity Abamectin. The method comprises the following steps: dissolving Abamectin coarse powder in acetone, loading a sample to a chromatographic column filled with octadecyl silane bonded silica gel inversed phase chromatography fillers, gradient eluting the sample by using mixed liquid of a polar solvent and water as eluent, and carrying out stepwise collection, liquid phase detection, mixing, concentration and drying to obtain the target product, the purity of Abamectin B1 in the target product is 98.5-99.5%, and the purity of Abamectin B1a is not larger than 97% while not smaller than 95%. The component proportions of Abamectin B1a and Abamectin B1b in the final product of the invention are controllable, B1b is not larger than 5.0%, the other impurities 1# to 9# are not larger than 0.1%, the process is simple, the yield is stable, the quality is controllable and safer technical support is provided for production of pharmaceutical grade raw materials.

Description

technical field [0001] The invention belongs to the technical field of industrial microbes, and in particular relates to a method for preparing high-purity abamectin with controllable component ratios by using crude abamectin. Background technique [0002] Avermectins (AVM), also known as Avermectins, are a group of macrolide antibiotics produced by the fermentation of Streptomyces avermitilis, which are C5, C22-C23 and C25 Eight homologues with different structures at three positions, namely 4 main components (Ala, A2a, B1a and B2a) and 4 minor components (A1b, A2b, B1b and B2b), the specific structures are as follows: [0003] ,in: . [0004] Abamectin is a class of macrolide antibiotics with a sixteen-membered ring structure that has insecticidal, acaricidal, and nematicidal activities. It has extremely strong killing activity against internal and external parasites, and has no antifungal and bacterial activity. , nor can it inhibit the synthesis of protein chitin, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/06
Inventor 杨德昌刘书琴高玉成张宾张丽强杨飞李学红王栋良
Owner NORTH CHINA PHARMA GROUP AINO
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