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目的:建立顶空气毛细管气相色谱法测定尼可刹米中甲苯残留量的方法。方法:采用顶空气毛细管气相色谱法,以水为溶解介质,色谱柱为DB-624石英毛细管柱,柱温110℃,检测器为FID,检测器温度为250℃,进样口温度为150℃。结果:甲苯浓度的线性范围为0.0178～0.89 mg·ml~(-1)(r=0.999 9);平均回收率为99.4%(RSD=1.1%);定量限为0.24μg·ml~(-1);3批样品中甲苯的残留量均符合《中国药典》2005年版要求。结论:方法操作简单,结果准确,可用于尼可刹米中甲苯残留量的测定。
OBJECTIVE: To establish a method for the determination of toluene in nikethamide by headspace capillary gas chromatography. Methods: The capillary column was DB-624 quartz capillary column with headspace capillary gas chromatography with water as the dissolution medium. The column temperature was 110 ℃, the detector was FID, the detector temperature was 250 ℃ and the inlet temperature was 150 ℃ . Results: The linear range of toluene concentration was 0.0178-0.89 mg · ml -1 (r = 0.999 9). The average recovery was 99.4% (RSD = 1.1%). The limit of quantification was 0.24 μg · ml -1 ). The residual amount of toluene in the three batches of samples all met the requirements of 2005 edition of Chinese Pharmacopoeia. Conclusion: The method is simple and accurate. It can be used for the determination of toluene residue in nichemamide.