An method of in situ derivatization-headspace gas chromatrograph-electron capture detecter was established to determine methyl methanesulfonate (MMS),ethyl methanesulfonate (EMS) and isopropyl methanesulfonate (IMS),known as potential genotoxic impurities in imatinib mesylate. An INOWAX (30 m×0.25 mm,1.0 μm) capillary column was used to separate and electron capture detecter (ECD) was used for quantitative determination. Sodium iodide was used as a derivatizing agent. Headspace sampling was conducted with a split ratio of 1:10. Calibration curves showed good linearity over the concentration range of 5~125 ng/mL for three of alkyls methanesulfonate. The results of limit of quantification of MMS,EMS and IMS were 5,2.5 and 2.5 ng/mL,respectively. Recoveries of MMS,EMS and IMS were 87.91%, 102.35% and 101.94%, respectively. The method showed satisfactory convenience, accuracy, repeatability and specificity.%建立了同时检测甲磺酸伊马替尼中甲磺酸甲酯、甲磺酸乙酯和甲磺酸异丙酯3种基因毒性杂质的原位衍生化顶空气相色谱法.采用Welch WM-INNOWAX(30 m×0.25 mm, 1 μm)色谱柱,电子捕获检测器(ECD),分流比20:1;碘化钠原位衍生化顶空进样.3种甲磺酸烷基酯在5~125 ng/mL的范围内线性关系良好,定量限分别为5、2.5和2.5 ng/mL,平均回收率分别为87.91%、102.35%和101.94%.该方法简便、准确、重现性好且专属性强.
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