HPLC-MS/MS法测定雷贝拉唑钠中的基因毒性杂质  

Determination of Genotoxic Impurity in Rebeprazole Sodium by HPLC-MS/MS

作　　者：郭跃龙[1] 张学智 GUO Yue-long;ZHANG Xue-zhi(Department of Pharmacy,Jiangsu Province Official Hospital,Nanjing 210024,China;Jiangsu Aosaikang Pharmaceutical Co.,Ltd.,Nanjing 211112,China)

机构地区：[1]江苏省省级机关医院药剂科,江苏南京210024 [2]江苏奥赛康药业有限公司,江苏南京211112

出　　处：《海峡药学》2020年第4期81-83,共3页Strait Pharmaceutical Journal

摘　　要：目的建立液相色谱-串联质谱联用方法测定雷贝拉唑钠中基因毒性杂质的含量。方法采用色谱柱Agilent Poroshell 120 C18(150mm×2.1mm,2.7μm),以0.01mol·L^-1乙酸铵-0.1%甲酸水溶液-甲醇为流动相,在电喷雾正离子模式下,对m/z 169.0608、m/z 212.1281和m/z 246.0891离子进行选择性监测。结果基因毒性杂质2,3-二甲基-4-硝基吡啶氮氧化物、2,3-二甲基-4-甲氧基丙氧基吡啶氮氧化物和2-氯甲基-3-甲基-4-(3-甲氧基丙氧基)吡啶盐酸盐氮氧化物,在限度浓度的5%~200%范围内,均与峰面积线性关系良好(r=1.0000);检测限依次为3.758pg、3.757pg和3.741pg,定量限依次为18.79pg、18.78pg和18.70pg;基因毒性杂质平均回收率(n=9)均在80%~120%之间(RSD<15%)。结论本方法操作简便,结果可靠,可用于雷贝拉唑钠中上述基因毒性杂质含量的检测。OBJECTIVE To establish an HPLC-MS analytical method for the determination of genotoxic impurity in rabeprazole sodium.METHODS Chromatographic separation was based on an Agilent Poroshell 120 C18(150 mm×2.1 mm,2.7μm) column using 0.01 mol·L^-1 ammonium acetate-0.1% formic acid-methanolas mobile phase in isocratic elution mode.Mass spectrometry was operated in positive ion mode.Mass spectrometry was operated in positive ion mode.Selective ion monitors were set at m/z 169.0608 for SM1-Imp2,m/z 212.1281 for SM1-Imp7 and m/z 246.0891 for SM1-Imp13.RESULTS Good linear correlations were observed in the range of 5%-200% limit concentration(r=1.0000) for SM1-Imp2,SM1-Imp7 and SM1-Imp13.The quantification limit at 18.79 pg,18.78 pg,18.70 pg and the detection limit at 3.758 pg,3.757 pg,3.741 pg respectively.Furthermore,the average recoveries were between 80%~120%(n=9,RSD<15%) for all.CONCLUSION The proposed method is simple and reliable,and quite suitable for the determination of SM1-Imp2,SM1-Imp7,SM1-Imp13 in Rabeprazole sodium.

关 键 词：雷贝拉唑钠 液相色谱质谱联用 基因毒性杂质 基因毒性杂质2 3-二甲基-4-硝基吡啶氮氧化物 2 3-二甲基-4-甲氧基丙氧基吡啶氮氧化物 2-氯甲基-3-甲基-4-(3-甲氧基丙氧基)吡啶盐酸盐氮氧化物 

分 类 号：R927[医药卫生—药学]