气相色谱法检测沙咪珠利中的残留溶剂

Determination of Methanol, Ethanol and Toluene in Acetamizuril by Gas ChromatographyWang Hao-xin, Wang Xiao-yang, Zheng Wen-li, Zhang Li-fang, Fei Chen-zhong, Zhang Ke-yu, Wang Mi, Li Tao, Xiao Sui, Xue Fei-qun

关键词:  残留溶剂  沙咪珠利  甲醇  乙醇  甲苯  气相色谱法。

Key words:  Residual organic solvent  Acetamizuril  Methanol  Ethanol  Toluene  Gas Chromatography.

摘要:

建立了同步测定沙咪珠利中甲醇、乙醇和甲苯残留溶剂的气相色谱法。采用DB-WAX（30 m×0.25 mm× 0.25 μm）毛细管柱，程序升温，初始60 ℃，保持4 min，50 ℃/min升至80 ℃，保持1 min，再以100 ℃/min升至200 ℃，保持4 min；载气为氮气，直接进样，测定残留溶剂含量。甲醇、乙醇和甲苯线性范围分别为31.68~506.8、18.96~758.4、8.64~138.7 μg/mL（R2：0.995 8~0.997 1），定量限分别为2.091、1.564、0.572 μg/kg，精密度RSD均小于5%，平均回收率为99.87%~100.39%。采用气相色谱方法可同时测定沙咪珠利中残留的甲醇、乙醇和甲苯的含量, 方法简便准确。

Abstract:

A GC–MS method was developed and validated for the detection and quantification of residual solvents of Acetamizuril. The method was validated for methanol, ethanol and toluene. The proposed method used a DB-WAX(30 m×0.25 mm× 0.25 μm) capillary column with an oven temperature program from 60 ℃ (held for 4 min) to 80 ℃(held for 1 min) at 50 ℃/min and then from 80 ℃ to 200 ℃(held for 4 min) at 100 ℃/min. The carrier gas was nitrogen, and the residual solvents were determined by direct injection. The studied ranges of methanol, ethanol and toluene were 31.68~506.8, 18.96~758.4, 8.64~138.7 μg/mL(R2: 0.995 8~0.997 1), the limit of quantification were 2.091, 1.564, 0.572 μg/kg, the RSD of precision were less than 5%, the average collection of preparation was in the range of 99.87%~100.39%. A method obtained for the quantification of residual solvents in Acetamizuril was simple and precise.