Avermectin；_高效液相色谱；_质谱；

Avermectin粗粉的结晶工艺研究与杂质分析

http://www.100md.com 《中国抗生素杂志》 2006年第1期

Avermectin；,高效液相色谱；,质谱；,杂质；,结晶,,Avermectin；,高效液相色谱；,质谱；,杂质；,结晶,1材料方法,结果与讨论,3结论,参考文献

     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B1a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。

    关键词： Avermectin；高效液相色谱；质谱；杂质；结晶

    Study on the crystallization of avermectin crude powder

    and its impurities analysis

    Liu Ji1,2, Ji Qingrong1, Chang Zhidong1, Xie Zhi1, Zhang Guifeng1,

    Shen Shufeng1, Sun Xinghua1, Lei Chao1 and Liu Huizhou1 (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)

    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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