HPLC-ESI-MS^n法分离和鉴定盐酸克林霉素棕榈酸酯原料药中的10种杂质  

HPLC-ESI-MS^n separation and identification of ten impurities in clindamycin palmitate hydrochloride drug substances

作　　者：王建 王红波[2] 洪利娅 

机构地区：[1]浙江省食品药品检验研究院,杭州310004 [2]浙江工业大学,杭州310014

出　　处：《药物分析杂志》2012年第12期2213-2220,共8页Chinese Journal of Pharmaceutical Analysis

基　　金：国家药典委员会国家药品标准提高研究项目(国药典化发[2010]84号)

摘　　要：目的:用HPLC-ESI-MSn法分离和鉴定国产盐酸克林霉素棕榈酸酯原料药中的10种杂质,并探讨这些杂质的质谱裂解规律。方法:采用Agilent ZORBAX SB-C8色谱柱(150 mm×3.0 mm,3.5μm),流动相为5 mmol.L-1醋酸铵溶液-乙腈(25∶75),在正离子检测方式下,AB SCIEX 4000 Q TRAP LC/MS/MS仪对盐酸克林霉素棕榈酸酯中的杂质进行在线多级质谱分析。结果:通过多级质谱裂解推断盐酸克林霉素棕榈酸酯原料药中10种杂质分别为克林霉素、丙叉克林霉素、亚砜克林霉素棕榈酸酯、克林霉素十二酸酯、棕榈酸乙酯、克林霉素十四酸酯、克林霉素B棕榈酸酯、表克林霉素棕榈酸酯、克林霉素十八酸酯、丙叉克林霉素棕榈酸酯。结论:鉴定了盐酸克林霉素棕榈酸酯原料药中10个杂质的结构,其中3个杂质为新的杂质。Objective：Ten impurities in clindamycin palmitate hydrochloride drug substances made in China were separated and identified by HPLC - ESI - MSn method. The fragmentation patterns and structural assignment of these impurities were studied, Methods： Agilent ZORBAX SB - C8 column （ 150 mm×3.0mm,3.5μm） was used with a mobile phase of 5 mmol · L^- 1 ammonium acetate solution -acetonitrile（25：75 ）. In positive mode, the impu- rities in clindamycin palmitate hydrochloride were analyzed by AB SCIEX 4000 Q TRAP LC/MS/MS. The complete fragmentation patterns of ten impurities were studied by MSn and used to obtain information about the structure of these impurities. Results：The ten impurities in clindamycin palmitate hydroehloride drug substances were deduced based on the HPLC -MSn data as clindamycin, anisylidene clindamycin, clindamycin palrnitate sulphoxides, clinda- mycin laurate, ethyl palmitate, clindamycin myristate, clindamycin B - palmitate, epiclindamycin palmitate, clinda- mycin stearate, anisylidene clindamycin palmitate. Conclusion： The structures of ten impurities in clindamycin pal- mitate hydrochloride drug substances were identified, of which three impurities were new impurities.

关 键 词：盐酸克林霉素棕榈酸酯 杂质结构 有关物质 高效液相串联多级质谱法 克林霉素 丙叉克林霉素 亚砜克林霉素棕榈酸酯 克林霉素十二酸酯 棕榈酸乙酯 克林霉素十四酸酯 克林霉素B棕榈酸酯 表克林霉素棕榈酸酯 克林霉素十八酸酯 丙叉克林霉素棕榈酸酯 杂质的控制和鉴定 标准提高 

分 类 号：R917[医药卫生—药物分析学]