HPLC-MS/MS法分析兰索拉唑中潜在基因毒性杂质  

Trace Determination of Potential Genotoxic Impurities in Lansoprazole by HPLC-MS/MS

作　　者：吴莉 仲艳 Wu Li;Zhong Yan(Center for Certification Evaluation&JSMPA,Nanjing 210002,China;Jiangsu KANION Pharmaceutical Co.Ltd.)

机构地区：[1]江苏省药品监督管理局审评中心,南京210002 [2]江苏康缘药业股份有限公司

出　　处：《中国药师》2022年第2期378-381,共4页China Pharmacist

摘　　要：目的:建立液相色谱-串联质谱法测定兰索拉唑中潜在基因毒性杂质的含量。方法:采用Agilent XDB-C_(18)色谱柱(50 mm×4.6 mm,1.8μm),以0.005 mol·L^(-1)乙酸铵缓冲液(A)∶乙腈(B)为流动相,梯度洗脱,流速0.5 ml·min^(-1),柱温30℃;采用ESI离子源,正离子模式下MRM采集,监测离子对m/z 386.6→119.1、m/z 402.1→119.1、m/z 370.1→320.5进行测定。结果:潜在基因毒性杂质Ⅰ、杂质Ⅱ、杂质Ⅲ在6~120 ng·ml^(-1)浓度范围内线性关系良好(r分别为0.9997,0.9985,0.9914),平均回收率分别为95.5%,94.9%,97.8%,RSD分别为6.9%,2.9%,5.8%(n=9);定量限分别为4.6,0.003,0.003 ng·ml^(-1)。结论:本方法操作简便,结果可靠,可用于兰索拉唑药物中潜在基因毒性杂质含量的同时测定。Objective:To establish an HPLC-MS/MS analytical method for the determination of potential genotoxic impurities in lansoprazole.Methods:The analytical column was Agilent XDB-C_(18)(50 mm×4.6 mm,1.8μm)with the mobile phase of 0.005 mol·L^(-1)ammonium acetate buffer and acetonitrile with gradient elution,and the flow rate was 0.5 ml·min^(-1).The column temperature was set at 30℃.The detection was achieved in an ESI positive ion mode with MRM.The MS was carried out by m/z 386.6→119.1,m/z 402.1→119.1 and m/z 370.1→320.5 for the determination of potential genotoxic impurities.Results:The calibration curves of impurityⅠ,ⅡandⅢwere in good linearity over the range of 6^(-1)20 ng·ml^(-1)(r=0.9997,0.9985 and 0.9914).The average recoveries were 95.5%,94.9%and 97.8%with the RSD of 6.9%,2.9%and 5.8%(n=9),respectively.The LOQs were 4.6,0.003 and 0.003 ng·ml^(-1),respectively.Conclusion:The established method is simple,rapid and reliable,which is applicable for the quantification of multiple potential genotoxic impurities in lansoprazole.

关 键 词：兰索拉唑 潜在基因毒性杂质 杂质Ⅰ、杂质Ⅱ、杂质Ⅲ 液相色谱-串联质谱 

分 类 号：R917[医药卫生—药物分析学]