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Method for separating and purifying moxidectin

A technology for separation and purification of moxidectin, which is applied in the field of separation and purification of macrolide antibiotics, can solve problems such as cumbersome process, and achieve the effect of simple operation, easy control and high purity

Active Publication Date: 2017-09-29
JIANGSU HANBON SCI & TECH CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a method for the separation and purification of moxidectin, which adopts a supercritical fluid chromatography system to separate and purify moxidectin, so as to solve the problems such as the cumbersome process existing in the process of purifying moxidectin at present

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0011] (1) Dissolve the crude moxidectin in acetonitrile, and then filter it with a 0.45 μm microporous membrane;

[0012] (2) Prepare methanol: ethanol: acetonitrile = 40:40:20 entrainer;

[0013] (3) Use a supercritical fluid chromatography system to separate and purify the filtered crude product. The specific method is: the size of the chromatographic column is Φ10×250mm, the column is equipped with bare silica gel filler, the particle size of the filler is 10μm, and the mobile phase is supercritical CO 2 : Entrainer = 88:12, flow rate 3ml / min, mobile phase system balance system 15min, inject 1g, start to receive the target component after elution for 60min, and then use supercritical CO 2 : The mobile phase of entrainer=60:40 carries out eluting impurity, adopts differential detector to detect, collects target fraction;

[0014] (4) The collected target fractions were concentrated by rotary distillation to obtain moxidectin, which was tested to have a purity of 96.8%.

Embodiment 2

[0016] (1) Dissolve the crude moxidectin in acetonitrile, and then filter it with a 0.45 μm microporous membrane;

[0017] (2) Prepare methanol: ethanol: acetonitrile = 38:38:24 entrainer;

[0018] (3) Use a supercritical fluid chromatography system to separate and purify the filtered crude product. The specific method is as follows: the size of the chromatographic column is Φ20×250mm, and the column is equipped with octadecylsilane bonded silica gel packing, the packing particle size is 15 μm, and the mobile phase is Supercritical CO 2 : Entrainer = 92:8, flow rate 12ml / min, mobile phase system balance system 15min, inject 5g, start to receive the target component after elution for 62min, and then use supercritical CO 2 : The mobile phase of entrainer=60:40 carries out eluting impurity, adopts differential detector to detect, collects target fraction;

[0019] (4) The collected target fractions were concentrated by rotary distillation to obtain moxidectin with a purity of 9...

Embodiment 3

[0021] (1) Dissolve the crude moxidectin in acetonitrile, and then filter it with a 0.45 μm microporous membrane;

[0022] (2) Prepare methanol: ethanol: acetonitrile = 35:35:30 entrainer;

[0023] (3) Use a supercritical fluid chromatography system to separate and purify the filtered crude product. The specific method is as follows: the size of the chromatographic column is Φ50×250mm, and the column is equipped with a diol-based silica gel filler with a particle size of 15 μm. The mobile phase is supercritical CO 2 : Entrainer = 96:4, flow rate 66ml / min, mobile phase system balance system 15min, sample injection 20g, start to receive the target component after elution 62min, and then use supercritical CO 2 : The mobile phase of entrainer=60:40 carries out eluting impurity, adopts differential detector to detect, collects target fraction;

[0024] (4) The collected target fractions were concentrated by rotary distillation to obtain moxidectin, which was tested to have a purit...

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PUM

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Abstract

The invention discloses a method for separating and purifying moxidectin. The method comprises the step of carrying out separation and purification to obtain the moxidectin of which the purity is 96% or above, wherein a supercritical fluid chromatographic system is adopted, a silica-gel-based filler is used as a stationary phase, supercritical CO2 is used as a mobile phase, and a mixture of methanol, ethanol and acetonitrile is used as an entrainer. The method for separating and purifying moxidectin is simple to operate; and more importantly, by using the supercritical CO2 as the mobile phase, only small amounts of organic solvents are added, thereby reducing the environmental pollution caused by organic solvents, and being green and environment-friendly.

Description

technical field [0001] The invention relates to a method for separating and purifying macrolide antibiotics, in particular to a method for purifying moxidectin. Background technique [0002] Moxidectin, alias moxidectin, English name is Moxidectin, white or off-white amorphous powder, almost insoluble in water, very soluble in ethanol (96%), slightly soluble in hexane, is a new type of anti Parasite medicine is a single-component macrolide antibiotic fermented by Streptomyces. [0003] Compared with other macrolide antiparasitic drugs such as ivermectin and avermectin, moxidectin has a single component, and has higher anthelmintic activity, long-term, and safety characteristics, especially for nematodes (adult worms) and larvae) and arthropods, it has good anti-insect activity at extremely low doses, and has high repelling activity against nematodes and arthropod parasites in dogs, cattle, sheep, and horses, and has been widely used to treat dairy cows, Internal and extern...

Claims

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Application Information

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IPC IPC(8): C07D493/22
CPCC07D493/22Y02P20/54
Inventor 陈海刘大伟张大兵韩海峰尤慧艳文卡特
Owner JIANGSU HANBON SCI & TECH CO
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