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 Chromatography

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（30m×0．25mm×0．25μm）毛细管柱，程序升温，初始60℃，保持4min，50℃／min升至80℃，保持1min。再以100℃／min升至200℃。保持4min；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、8．64～138．7μg/mL（R^2：0．9958～0．9971），定量限分别为2．091、1．564、0．572μg／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。

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×0.25mm×0.25μm） capillary column with an oven temperature program from 60℃ （held for 4 min） to 80℃ （held for 1 rain） at 50 ℃/min and then from 80 ℃ to 200℃ （held for4 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 p,g/mL（R^2 ： 0.9958-0.9971） , 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%- residual solvents in acetamizuril was simple and precise. 100.39%. A method obtained for the quantification of residual solvents in acetamizuril was simple and precise.