HPLC-MS法分析甲苯磺酸拉帕替尼中痕量基因毒性杂质

发布时间：2019-06-14 06:35

【摘要】：目的:建立液相色谱-质谱联用方法测定甲苯磺酸拉帕替尼中基因毒性杂质的含量。方法:采用色谱柱C18(4.6 mm×250 mm,5μm),以0.1%甲酸溶液-乙腈(20∶80)为流动相,流速1.0 m L·min-1,电喷雾离子化(ESI)正离子模式下选择m/z252离子进行检测。结果:基因毒性杂质4-(3-氟苯甲氧基)-3-氯苯胺质量浓度在0.08~8 ng·m L-1范围内,与峰面积线性关系良好(r=1.000);检测限为0.003 6 ng,定量限为0.010 7 ng;样品中基因毒性杂质测定结果的重复性良好,RSD(n=6)为7.5%;基因毒性杂质平均回收率(n=9)为96.6%。结论:本方法操作简便,结果可靠,可以用于甲苯磺酸拉帕替尼中基因毒性杂质4-(3-氟苯甲氧基)-3-氯苯胺含量的检测。
[Abstract]:Objective: to establish a liquid chromatography-mass spectrometry (LC-MS) method for the determination of genotoxic impurities in rapatinib toluene sulfonate. Methods: C _ (18) column (4.6 mm 脳 250 mm, 5 渭 m) was used, 0.1% formic acid solution-acetonitrile (20:80) was used as mobile phase, the flow rate was 1.0 mL 路min-1, and m/z252 ion was selected under electrospray ionization (ESI) positive ion mode. Results: the linear range of genotoxic impurity 4-(3-fluorobenzoxyl)-3-chloranilide was 0.08 ng 路mL 鈮，

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