论文部分内容阅读
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N’N-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Wonda CAPWAX毛细管柱为色谱柱,程序升温,N2为载气,载气流速为4.0m L·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%,n=9),定量限分别为0.20、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。
OBJECTIVE: To establish a capillary gas chromatographic method for the simultaneous determination of three residual organic solvents, methanol, ethanol and DMF in the commercial imatinib mesylate. Methods: Wonda CAP WAX capillary column was used as the chromatographic column. The temperature was programmed and N2 was the carrier gas. The flow rate of carrier gas was 4.0? M L?? Min-1. The temperature of the detector was 250? , The inlet temperature is 200? ℃, the injection volume is 1.0? ΜL. Using n-butanol as the internal standard, the residual amount of the three organic solvents in the sample was calculated by internal standard method. Results: Methanol, ethanol and DMF could be completely separated under the established chromatographic conditions. The linearity was good in the range of 2.94 ~ 44.11, 4.91 ~ 73.68 and 0.084 ~ 12.60? Mg? · L-1 respectively = 0.9940 ~ 0.9985). The average precision of RSD was less than 5.0% (n = 6) and the average recoveries were 104.8% -105.8% (RSD <5.0%, n = 9) And 0.08 ng (signal to noise ratio of 10: 1). The detection limits were 0.05, 0.11 and 0.02 ng respectively (signal to noise ratio of 3: 1). No methanol and DMF were detected in the sample and the ethanol content was below the relevant limit. Conclusion: The method is simple, accurate, sensitive and reproducible. It can be used for the determination of residual organic solvents in imatinib mesylate APIs.