顶空进样GC-SIM-MS测定硝唑尼特中溶剂残留甲醇含量

摘要

利用气相色谱-选择离子监测质谱联用仪( GC-SIM-MS)测定硝唑尼特样品中溶剂残留甲醇的含量,顶空进样,温度为70℃,时间为20 min. SIM定量离子m/z 32,参考离子m/z 31,30和29.甲醇质量浓度在0.5~100μg/mL内呈良好的线性(R2=0.99992).方法相对标准偏差为2.49%~4.85%,样品加标回收在94.5%~102.8%之间,检测限为0.5μg/mL,符合定量分析的要求.%The determination of methanol solvent residues in the samples of nitazoxanide using gas chromatography-selected ion monitoring-mass spectrometry( GC-SIM-MS) has been curried out. A peak area standard curve method is used as the quantitative method. The heating temperature of the sample was 70 ℃,with an equilibrium time of 20 min, SIM m/z 32, m/z 31, 30, and 29. The concentration of toluene was linear in the range of 0. 5~100 μg /mL (R2=0. 999 92). The relative standard deviation of the method was 2. 49% ~4. 85%, the recovery was between 94. 5% ~102. 8%, the detection limit was 0. 5 μg/mL, which were in accordance with the requirement of quantitative analysis.