毛细管气相色谱法测定甲磺酸伊马替尼中残留有机溶剂

目的：建立可同时测定甲磺酸伊马替尼原料药中甲醇、乙醇和NN-二甲基甲酰胺（DMF）等3种残留有机溶剂的毛细管气相色谱法。方法：采用WondaCAPWAX毛细管柱为色谱柱，程序升温，N2为载气，载气流速为4，0mL·min^-1，氢火焰离子化检测器，检测器温度为250℃，进样口温度为200℃，进样量为1．0μL。以正丁醇为内标，通过内标法计算样品中3种有机溶剂残留量。结果：甲醇、乙醇和DMF在所建立的色谱条件下均能完全分离，分别在2．94-44，11、4．91-73．68和0．084-12．60mg·L^-1。的质量浓度范围内线性关系良好（r=0．9940-0．9985），进样精密度（RSD）均小于5．0％（n=6）．平均回收率为104．8％-105．8％（RSD〈5，0％，，7：9），定量限分别为O．20、0．33和0．08ng（信噪比为10：1），检测限分别为0．05、0．11和0．02ng（信噪比为3：1）。样品中未检出甲醇和DMF，乙醇含量低于有关限度规定。结论：该方法简便、准确、灵敏、重复性好．可用于甲磺酸伊马替尼原料药中残留有机溶剂的检测。

Determination of Residual Organic Solvents in lmatinib Mesylate by Capillary GC

To establish a capillary GC method for simultaneous determination of methanol, ethanol and N,N-dimethylformamide（DMF） as residual organic solvents in imatinib mesylate API. WondaCAP WAX capillary column with temperature programming, nitrogen as carrier gas at a flow rate of 4.0 mL · min^-1 and FID at 250 ℃ were used with an injection port tenaperaturc of 200 ℃ and an injection volume of 1.0μL. With n-butyl alcohol as internal standard, three kinds of organic solvent residues in the samples were calculated by internal standard method. Methanol, ethanol and DMF were completely separated under the established chromatographic condition. Good linearities were obtained in corresponding concentration ranges of 2.94-44.1 t mg· L-^-1（methanol）, 4.91-73.68 mg· L^-1（ethanol ） and 0.084-12.60 mg· L^-1（DMF）, with correlation coefficients of 0.9940-0.9985. The sampling precisions （RSDs） were less than 5.0%（n=6）. The average recovery rates were 104.8%-105.8%（RSD〈5%, n=9）. The limits of quantification for them were 0.20, 0.33 and 0.08 ng respectively（ S/N= 10 ： 1）. The limits of detection lbr them were 0.05, 0.11 and 0.02 ng respectively（S/N=3： 1）. Methanol and DMF were not detected and ethanol contents were below the limit of regulation in the samples. The method is simple, accurate, sensitive and repeatable. It is suitable for the determination of the residual organic solvents in imatinib mesylate API.