【摘要】：目的:建立液相色譜-質(zhì)譜聯(lián)用方法測定甲苯磺酸拉帕替尼中基因毒性雜質(zhì)的含量。方法:采用色譜柱C18(4.6 mm×250 mm,5μm),以0.1%甲酸溶液-乙腈(20∶80)為流動相,流速1.0 m L·min-1,電噴霧離子化(ESI)正離子模式下選擇m/z252離子進(jìn)行檢測。結(jié)果:基因毒性雜質(zhì)4-(3-氟苯甲氧基)-3-氯苯胺質(zhì)量濃度在0.08~8 ng·m L-1范圍內(nèi),與峰面積線性關(guān)系良好(r=1.000);檢測限為0.003 6 ng,定量限為0.010 7 ng;樣品中基因毒性雜質(zhì)測定結(jié)果的重復(fù)性良好,RSD(n=6)為7.5%;基因毒性雜質(zhì)平均回收率(n=9)為96.6%。結(jié)論:本方法操作簡便,結(jié)果可靠,可以用于甲苯磺酸拉帕替尼中基因毒性雜質(zhì)4-(3-氟苯甲氧基)-3-氯苯胺含量的檢測。
[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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