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A method for separating and purifying naimamectin by high performance liquid chromatography

A high-performance liquid chromatography and naimectin technology, which is applied in the field of high-performance liquid chromatography for purifying moxidectin precursor naimactin, can solve the problems of high cost, large proportion of organic solvents, complicated procedures and the like, and achieves the The effect of shortened production cycle, short purification time and fewer process steps

Active Publication Date: 2017-12-26
CHANGSHU NANOMICRO BIOTECHNOLOGY CO LTD
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  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

[0010] In these existing technologies, some purification schemes can only obtain crude neimamectin with lower purity, and the purity of the product cannot meet the requirements for the subsequent efficient production of moxidectin, so its purity needs to be further improved to meet the requirements
Some have complex procedures, which require many steps such as decolorization, extraction, and adsorption, and the volume of eluent used is large, the proportion of organic solvents is large, and the cost is high, which has a certain impact on the human body and the environment. Therefore, it is necessary to further reduce the process. and the amount of organic solvents, in order to achieve pure neimamectin with environmental friendliness, high purity and high recovery rate to meet subsequent requirements

Method used

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  • A method for separating and purifying naimamectin by high performance liquid chromatography
  • A method for separating and purifying naimamectin by high performance liquid chromatography
  • A method for separating and purifying naimamectin by high performance liquid chromatography

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Embodiment 1

[0032] Purification of naimamectin: using a (4.6×250)mm chromatographic column, UniPS 30-300 (polystyrene-divinylbenzene copolymer particle size 30±1.5μm, Suzhou Nanoway Technology Co., Ltd.) as the separation The filler is purified, the column volume is 4.1ml, and the column is equilibrated with 68-72% acidic ethanol aqueous solution. The mobile phase A is an aqueous hydrochloric acid solution with a pH value of 2 to 3, and the mobile phase B is ethanol with a pH of 2 to 3. Different percentages of the mobile phase A and mobile phase B are used to form the mobile phase used for elution. The crude product of naimamectin (purity 65-68%) is firstly dissolved with ethanol aqueous solution, mixed and then filtered with a 0.45 μm filter membrane. The concentration is 100mg / ml, the sample volume is 0.42ml, and the sample volume is about 10mg / ml. The sample loading flow rate is 1ml / min, first use 68-72% acidic ethanol aqueous solution to wash 9-10 column volumes, and 78-80% acidic e...

Embodiment 2

[0034] Purification of naimamectin: using a (4.6×250)mm chromatographic column, UniPS 40-300 (polystyrene-divinylbenzene copolymer particle size 40±1.5μm, Suzhou Navi Technology Co., Ltd.) as the separation The filler is purified, the column volume is 4.1ml, and the column is equilibrated with 68-72% acidic ethanol aqueous solution. The mobile phase A is an aqueous acetic acid solution with a pH value of 2 to 3, the mobile phase B is ethanol with a pH of 2 to 3, and the mobile phase is a mixture of ethanol and acetic acid solutions in different proportions. The crude product of naimamectin (purity 65-68%) is firstly dissolved with ethanol aqueous solution, mixed and then filtered with a 0.45 μm filter membrane. The concentration is 100mg / ml, the sample volume is 0.42ml, and the sample volume is about 10mg / ml. The sample loading flow rate is 1ml / min, first use 68-72% acidic ethanol aqueous solution to wash 9-10 column volumes, and 78-80% acidic ethanol aqueous solution to elut...

Embodiment 3

[0036] Purification of naimamectin: adopt (4.6×250) mm chromatographic column, NM 100 filler (polystyrene-divinylbenzene copolymer, microsphere particle size 50-150 μm, pore size Suzhou Nawei Technology Co., Ltd.) was used as a separation and purification filler, with a column volume of 4.1 ml, and the column was equilibrated with 72% acidic ethanol aqueous solution. The mobile phase A is a hydrochloric acid solution with a pH of 2-3, and the mobile phase B is ethanol with a pH of 2-3. The crude product of naimamectin (purity 65-68%) is firstly dissolved with ethanol aqueous solution, mixed and then filtered with a 0.45 μm filter membrane. The concentration is 100mg / ml, the sample volume is 0.42ml, and the sample volume is about 10mg / ml. The sample loading flow rate is 1ml / min, first use 72% acidic ethanol aqueous solution to wash 9-10 column volumes, 78-80% acidic ethanol aqueous solution to elute target components for 6-7 column volumes, and finally use 90%- 95% acidic eth...

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Abstract

The invention provides a method for separating and purifying nemadectin by using the HPLC (high performance liquid chromatography). The method is implemented by taking styrene-divinylbenzene crosslinked microspheres as chromatographic packing through the steps that after a nemadectin coarse product solution is loaded in a chromatographic column, nemadectin adsorbed on the packing is eluted by using an acidic alcohol aqueous solution as a mobile phase. The method disclosed by the invention not only can achieve the high-purity and high-recovery-rate separation and purification of nemadectin, but also is small in mobile phase application amount, short in purification time and less in process step, so that the production cycle is greatly shortened.

Description

technical field [0001] The invention relates to a purification method, in particular to a method for purifying the moxidectin precursor neimamectin by high performance liquid chromatography. Background technique [0002] As the demand for antiparasitic drugs continues to grow, it is an indispensable technical requirement to obtain high-purity and high-efficiency antiparasitic drugs. [0003] Moxidectin (Moxidectin) is a new type of anti-parasitic macrolide third-generation abamectin drug, which has higher fat solubility and water solubility, and its metabolites in plasma are higher than those of other abamectins. Vermectin drugs, such as ivermectin and doramectin, are high in concentration and stay in the body for a long time, so the drug effect lasts longer. They can be safely injected into cattle, sheep, and camels to prevent internal and external parasites. In order to efficiently produce moxidectin, nemadectin with high purity and high recovery must be obtained first. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D493/22
CPCC07D493/22
Inventor 江必旺王燕李学宁吴俊成陈荣姬潘毅
Owner CHANGSHU NANOMICRO BIOTECHNOLOGY CO LTD
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