郑州大学学报（理学版）2019，Vol.51Issue(3)：104-108,5.DOI:10.13705/j.issn.1671-6841.2018240
顶空-气相色谱-质谱法同时测定7种甲磺酸酯类杂质
Simultaneous Determination of Seven Methanesulfonate Impurities by Headspace-GC-MS
摘要
Abstract
A procedure for the simultaneous determination of seven methanesulfonate genotoxic impuri-ties, such as MMS, EMS, i-PMS, n-PMS, s-BMS, i-BMS, n-BMS, employed in drug synthesis was de-veloped and validated by derivatization-headspace-GC-MS. The effects of type and amount of organic phase, reaction temperature and time related to the derivatization were studied and the optimum condi-tions were determined. The conditions including heating temperature and equilibration time to the head-space method were discussed and optimized, too. The methodological validation showed the good linearity for all the analytes with the correlation coefficients greater than 0.999 0, the detection limits ( S/N=3) varying from 0.21 to 2.64 μg/L, and the limits of quantitation ( S/N=10) from 0.70 to 8.81 μg/L. The standard deviations of intra-day and inter-day were less than 10.3% and 5.07% respectively, and the re-coveries of standard addition ranged from 88.2% to 115.1%. The method was successfully used to test te-bipenem intermediates and it was found that all the samples tested contained MMS, EMS and n-PMS. The method was suitable for the simultaneous analysis of the methanesulfonate impurities in active substances.关键词
烷基甲磺酸酯/衍生/顶空-气相色谱-质谱/检测Key words
alkyl methanesulfonate/derivatization/headspace-GC-MS/determination分类
医药卫生引用本文复制引用
王少敏,牛颖,代敏,魏一,刘宏民..顶空-气相色谱-质谱法同时测定7种甲磺酸酯类杂质[J].郑州大学学报（理学版）,2019,51(3):104-108,5.基金项目
国家自然科学基金项目(21772180). （21772180）
