Avermectin粗粉的结晶工艺研究与杂质分析VIP免费

下载后可任意编辑Avermectin 粗粉的结晶工艺讨论与杂质分析 作者：刘吉 季清荣 常志东，谢智 张贵峰 申淑锋 孙兴华 雷超 刘会洲【关键词】 Avermectin；,高效液相色谱；,质谱；,杂质；,结晶 摘要： 采纳高效液相色谱(HPLC)电喷雾串级质谱(ESIMSMS)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，下载后可任意编辑其中 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 ABSTRACT Avermectin crude powder 下载后可任意编辑were purified by crystallization and its impurities were identified by HPLC (high performance liquid chromatography)ESIMSMS (electrospraymass spectrometrymass 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 下载后可任意编辑structures to B1a. Recrystallizaton using methanol, ethanol, nbutanol and acetone as solvents were done respectively and it was found that methanol and nbutanol were good solvents for the separation of impurities. The impurities could be selectively separated using methanol or acetone. KEY WORDS Avermectin; HPLC; Mass spectrometry; Impurities; 下载后可任意编辑Crystallization Avermectin 是十六元大环内酯类抗生素，具有很强的杀虫活性，是一种良好的杀螨虫、昆虫和寄生虫的药物，可以用于人、畜和农作物。将 avermectin 粗粉重结晶三次，比较各次结晶的纯度及杂质的去除状况。乙醇为结晶溶剂，根据程序降温方法冷却结晶［9］；结晶过程中搅拌速度：150r/min，降温区间为 65℃～21℃，晶体纯度采纳 HPLC 分析，由面积归一化法...