UPLC-MS-MS法测定原料药中对甲苯磺酸酯类遗传毒性杂质  

Determination of P-toluenesulfonic Acid Esters Impurities in API by UPLC-MS/MS

作　　者：勾新磊[1] 徐双双[1] 赵婷[1] 张梅[1] 刘伟丽[1] 高峡[1] 赵新颖[1] 胡光辉[1] GOU Xin-lei;XU Shuang-shuang;ZHAO Ting;ZHANG Mei;LIU Wei-li;GAO Xia;ZHAO Xin-ying;HU Guang-hui(Beijing Key Laboralory of Organic Materials Testing Technology&Quality Evaluation,Beijing Centre for Physical and Chemical Analysis,Beijing 100089,China)

机构地区：[1]北京市理化分析测试中心,有机材料检测技术与质量评价北京市重点实验室,北京100089

出　　处：《广州化工》2020年第21期109-110,138,共3页GuangZhou Chemical Industry

基　　金：改革与发展专项(2020ZL0304)。

摘　　要：建立超高效液相色谱-串联质谱法(UPLC-MS/MS)测定硫酸氢氯吡格雷中对甲苯磺酸甲酯和对甲苯磺酸乙酯。以0.1%甲酸水-乙腈为流动相进行线性梯度洗脱。采用ESI离子源正离子模式,多反应监测模式下以外标法对2种遗传毒性杂质进行定量测定。2种遗传毒性杂质质量浓度在5.0~200.0 ng·mL^-1范围内线性关系良好;低中高加标回收率(n=3)为94.1%~105.3%,RSD为1.7%~4.4%。本方法操作简便,结果可靠,可用于硫酸氢氯吡格雷中对甲苯磺酸酯类遗传毒性杂质的检测。An UPLC-MS/MS analytical method for the determination of genotoxic impurities(methyl p-toluenesulfonate and ethyl p-toluenesulfonate)in clopidogrel bisulfate was established.The separation was performed with the mobile phase consisting of 0.1%formic acid aqueous solution and acetonitrile.Multiple reaction monitoring(MRM)was performed on a triple quadrupole mass spectrometer equipped with a ESI source in the positive mode.The calibration curve was linear for other compounds in the range of 5.0~200.0 ng·mL^-1.The recoveries(n=3)of adding concentrations were 94.1%~105.3%,RSD were 1.7%~4.4%.The established method is simple,rapid and reliable,which is applicable for both quantification of two genotoxic impurities in in clopidogrel bisulfate.

关 键 词：超高效液相色谱-串联质谱 遗传毒性杂质 对甲苯磺酸甲酯 对甲苯磺酸乙酯 

分 类 号：R917[医药卫生—药物分析学]