LC-MS/MS法检测盐酸鲁拉西酮中磺酸酯基因毒杂质  

Limit Test of Trace Amount of Genotoxic Substance-sulfonic Acid Ester in Lurasidone Hydrochloride by Liquid Chromatography Tandem Mass Spectrometry

作　　者：龚心实[1] 张斐[2] 董静[2] 刁旭[2] 李薇[2] 杭太俊[1] 

机构地区：[1]中国药科大学药分教研室,南京210009 [2]江苏先声药业有限公司,南京210042

出　　处：《药学与临床研究》2013年第3期235-238,共4页Pharmaceutical and Clinical Research

摘　　要：目的:采用LC-MS/MS法检查盐酸鲁拉西酮中的痕量磺酸酯基因毒杂质。方法:采用Waters Atlantis T3(2.1 mm×50 mm,3μm)色谱柱,10 mmol·L-1醋酸铵水溶液(55%)和甲醇(45%)作为流动相,等度洗脱,Agilent 1200色谱系统和Agilent 6460 MS/MS(ESI源)检测磺酸酯。结果:磺酸酯在0.05 ng·mL-1至25.00 ng·mL-1范围内线性良好,r>0.999,加样回收率为85%～115%,样品溶液在恒温进样盘(4℃)中6 h稳定。结论:该方法灵敏度高、准确度良好,可用于盐酸鲁拉西酮中磺酸酯基因毒杂质的定量检测,并为质量控制提供参考。Objective：To establish an LC-MS/MS method for the limit test of trace amount of genotoxic substance-sulfonic acid ester in lurasidone hydrochloride.Methods：The separation was achieved on a Waters Atlantis T3（2.1 mm×50 mm,3 μm） column.The mobile phase was 10 mmol.L-1 ammonium acetate solution and methanol at the proportion of 55 ∶45（v/v）.The Agilent 1200 liquid chromatographic system coupled with Agilent 6460 MS/MS was used to detect the sulfonic acid ester（ESI source,in MRM positive mode）.Results：The sulfonic acid ester showed good linearity at the range of 0.05～25.00 ng.mL-1,and the correlation coefficient was over 0.999.The sample recoveries were within 85% ～115%,and the sample solutions were stable in the auto-sampler within 6 hours.Conclusion：This simple,sensitive,reproducible method can be applied to test genotoxic sulfonic acid ester in lurasidone hydrochloride.

关 键 词：基因毒 LC-MS MS 磺酸酯 质量控制 

分 类 号：R927.1[医药卫生—药学] R991