| Avermectin粗粉的结晶工艺研究与杂质分析 |
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| 引用本文： | 刘吉,季清荣,常志东,谢智,张贵峰,申淑锋,孙兴华,雷超,刘会洲.Avermectin粗粉的结晶工艺研究与杂质分析[J].中国抗生素杂志,2006,31(1):45-48,51. |
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| 作者姓名： | 刘吉 季清荣 常志东 谢智 张贵峰 申淑锋 孙兴华 雷超 刘会洲 |
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| 作者单位： | 1. 中国科学院过程工程研究所分离科学与工程实验室,生化工程国家重点实验室,北京,100080;中国科学院研究生院,北京,100080
2. 中国科学院过程工程研究所分离科学与工程实验室,生化工程国家重点实验室,北京,100080 |
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| 基金项目： | 中国科学院资助项目;国家创新研究群体科学基金 |
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| 摘 要： | 采用高效液相色谱（HPLC）-电喷雾串级质谱（ESI-MS-MS）的方法对avermectin粗粉中的杂质进行定性分析。确定了主要杂质成分为：与Bla结构相类似的B1b、A1a、A1b、A2a、A2b、B2a 6个组份，其中A1a、B1b、B2a多次结晶也不易去除。随后考察了avermectin粗粉在甲醇、乙醇、正丁醇和丙酮中的重结晶，甲醇和正丁醇对杂质的去除效果更好；乙醇与丙酮相当，但对杂质去除的选择性不同。
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| 关 键 词： | 高效液相色谱 质谱 杂质 结晶 |
| 文章编号： | 1001-8689（2006）01-0045-04 |
| 收稿时间： | 2005-07-07 |
| 修稿时间： | 2005-07-072005-08-15 |
Study on the crystallization of avermectin crude powder and its impurities analysis |
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| Liu Ji,Ji Qing-rong,Chang Zhi-dong,Xie Zhi,Zhang Gui-feng,Shen Shu-feng,Sun Xing-hua,Lei Chao,Liu Hui-zhou.Study on the crystallization of avermectin crude powder and its impurities analysis[J].Chinese Journal of Antibiotics,2006,31(1):45-48,51. |
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| Authors: | Liu Ji Ji Qing-rong Chang Zhi-dong Xie Zhi Zhang Gui-feng Shen Shu-feng Sun Xing-hua Lei Chao Liu Hui-zhou |
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| Institution: | 1 .Laboratory of Separation Science and Engineering, State Key Laboratory of Biochemical Engineering, Institute of Process Engineering, Chinese Academy of Sciences, Beijing 100080; 2 .Graduate School of the Chinese Academic of Sciences, Beijing 100080 |
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| Abstract: | Avermectin crude powder were purified by crystallization and its impurities were identified by HPLC(high performance liquid chromatography)ESI-MS-MS(electrospray-mass spectrometry-mass spectrometry).Main impurities in crude powder were B1b,A1a,A1b,A2a,A2b and B2a,which were similar to B1a in structure.The separation of A1a,B1b and B2a was very difficult due to their greatly similar structures to B1a.Recrystallizaton using methanol,ethanol,n-butanol and acetone as solvents were done respectively and it was found that methanol and n-butanol were good solvents for the separation of impurities.The impurities could be selectively separated using methanol or acetone. |
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| Keywords: | Avermectin |
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