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A kind of separation and purification method of doramectin

A doramectin, separation and purification technology, applied in chemical instruments and methods, organic chemistry, preparation of sugar derivatives, etc., can solve problems such as inability to meet drug quality requirements, unfavorable industrial production, and low product purity, and achieve production costs. Low, environmentally friendly, simple process effect

Active Publication Date: 2018-03-27
CHONGQING QIANTAI BIOLOGICAL MEDICINE +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The first two documents only studied the extraction process of the product. Although the third document purified the product through steps such as resin and silica gel chromatography, the product had a low purity of only 92%, which could not meet the quality requirements of the drug; At the same time, due to the use of resin and silica gel chromatography, the yield is also low, the total yield is about 60%, and the production cost is high, which is not conducive to industrial production

Method used

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  • A kind of separation and purification method of doramectin
  • A kind of separation and purification method of doramectin

Examples

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Embodiment 1

[0030] Take 20L doramectin fermentation broth (fermentation unit 1.1 g / L, HPLC spectrum as figure 1 shown), add 800g of diatomaceous earth, stir evenly, and filter with a plate and frame filter press to obtain 6.3kg of filter residue. Add 18.9L of 95% methanol, keep the temperature at 50°C, stir for 8 hours, filter with suction, wash the filter cake with 4L of 95% ethanol, and collect about 22L of filtrate. Control the temperature at 50°C, concentrate the filtrate to a paste, the weight of the extract is about 58g, dissolve the extract with 2.3L of 65% ethanol, then add 46g of activated carbon, control the temperature at 50°C, stir for 2 hours, filter with suction, and use 200mL of 65% Wash the filter cake with ethanol, collect 2.5L of filtrate, add purified water to the filtrate continuously at a speed of 75ml per minute to dilute, stir while diluting until the ethanol concentration in the solution reaches 33%, then cool down while stirring until the temperature drops to 10...

Embodiment 2

[0032]Take 20L of doramectin fermentation broth (fermentation unit: 1.1g / L), add 400g of perlite, stir evenly, filter with a plate and frame filter press, and obtain 6.1kg of filter residue. Add 12.6L of 90% ethanol, keep the temperature at 40°C, stir for 5 hours, filter with suction, wash the filter cake with 4L of 90% ethanol, and collect about 16L of filtrate. Control the temperature at 40°C and concentrate the filtrate to a paste under reduced pressure. The weight of the extract is about 46g. Dissolve the extract with 920ml of methanol with a concentration of 60%, then add 69g of activated carbon, control the temperature at 50°C, stir for 2 hours, and filter with suction. The filter cake was washed with 100mL of 60% methanol, the filtrate was collected, and purified water was continuously added to the filtrate at a rate of 10ml per minute, and stirred while diluting until the methanol concentration of the solution reached 30%, and then cooled while stirring until the temper...

Embodiment 3

[0034] Take 20L of doramectin fermentation broth (fermentation unit 1.1 g / L), add 1600g of diatomaceous earth, stir evenly, filter with a plate and frame filter press, obtain 6.7kg of filter residue, heat and dry at 50°C to obtain dry bacterial residue About 2.72 kg, add 13.6L butyl acetate, keep the temperature at 60°C, stir for 15 hours, filter with suction, wash the filter cake with 4L butyl acetate, and collect about 17.5L of filtrate. Control the temperature at 60°C and concentrate the filtrate to a paste under reduced pressure. The weight of the extract is about 42g. Dissolve the extract with 2.1L of 70% acetone, then add 25g of activated carbon, control the temperature at 50°C, stir for 2 hours, and filter with suction. Wash the cake with 100mL of 70% acetone, collect 2.2L of filtrate, add purified water continuously to the filtrate at a rate of 110ml per minute, stir while diluting until the concentration of acetone in the solution reaches 35%, then cool down while stir...

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Abstract

The invention discloses a separation and purification method of doramectin. The method comprises the following steps: separating doramectin from fermentation liquor by extraction; then, decoloring by virtue of active carbon; and performing steps such as a programmed cooling crystallization method and the like to obtain a high purity doramectin product. The method disclosed by the invention has the advantages that doramectin is separated and purified by adopting the programmed cooling crystallization method, so that the method is high in product yield and purity, simple and feasible in process, low in production cost and suitable for industrial production.

Description

technical field [0001] The invention belongs to the field of medicinal chemistry, and in particular relates to a separation and purification method of doramectin. Background technique [0002] Doramectin (DRM) is the third-generation derivative of the macrolide antibiotic abamectin, produced by Streptomyces avermitilis ( Streptomyces avermitilis ) genetically engineered mutant strains were biosynthesized by adding cyclohexyl carboxylic acid to obtain a sixteen-membered macrolide semi-synthetic antibiotic, and the difference from ivermectin was in C 25 There is a cyclohexyl group in the position. The chemical name is 25-cyclohexyl-5-O-demethyl-25-de(1-methylpropyl) abamectin B1, and its chemical nature belongs to macrolide antibiotics, and its molecular formula is C 50 h 74 o 14 , Molecular weight is 899.11, melting point: 116°C-119°C, high fat solubility, easily soluble in organic solvents, such as methanol, ethanol, acetone, 1,2-propylene glycol, ethyl acetate, dimethyl...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07H17/08C07H1/08
CPCC07H1/08C07H17/08
Inventor 袁建栋刘省伟郭明唐恒杨久林
Owner CHONGQING QIANTAI BIOLOGICAL MEDICINE
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