顶空进样GC-SIM-MS测定硝唑尼特中溶剂残留甲醇含量

Determination of Methanol Solvent Residue in Nitazoxanide with Headspace GC-SIM-MS

  • 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20min.SIM定量离子m/z32, 参考离子m/z31, 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.关键字:硝唑尼特; 甲醇; 顶空进样; 气相色谱-选择离子监测质谱联用仪

     

    Abstract: 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.

     

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