Averm ectin粗粉的结晶工艺研究与杂质分析  

Study on the crystallization of avermectin crude powder and its impurities analysis

作　　者：刘吉[1] 季清荣[1] 常志东[1] 谢智[1] 张贵峰[1] 申淑锋[1] 孙兴华[1] 雷超[1] 刘会洲[1] 

机构地区：[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

出　　处：《中国抗生素杂志》2006年第1期45-48,51,共5页Chinese Journal of Antibiotics

基　　金：国家自然科学基金;创新研究群体基金(NO.20406021;NO.20236050和NO.20221603)联合资助

摘　　要：采用高效液相色谱(HPLC)-电喷雾串级质谱(ES I-M S-M S)的方法对averm ectin粗粉中的杂质进行定性分析。确定了主要杂质成分为:与B 1a结构相类似的B 1b、A 1a、A 1b、A 2a、A 2b、B 2a 6个组份,其中A 1a、B 1b、B 2a多次结晶也不易去除。随后考察了averm ectin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。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 to Bla in structure. The separation of A1a, Blb 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.

关 键 词：AVERMECTIN 高效液相色谱 质谱 杂质 结晶 

分 类 号：TQ465.5[化学工程—制药化工]