工作场所空气中异氰酸甲酯的高效液相色谱测定法

Determination of methyl isocyanate （MIC） in air of workplaces by HPLC

目的建立工作场所空气中异氰酸甲酯（MIC）的高效液相色谱测定方法。方法空气中蒸气态的MIC用浸渍过l-2-吡啶基哌嗪（1-2PP）的XAD-7管采集，MIC与荧光衍生剂1-2PP反应，在XAD．7管上生成稳定的荧光化合物，用乙腈解吸，经色谱柱分离，荧光检测器检测。结果该法在0．01-10μg／ml范围内呈线性关系，检出限为5．3×10^-4μg／ml；定量下限为O．01μg／ml；最低检出浓度为3．3×10^-3mg／m^3（以采集3L空气样品计），相对标准偏差为2．2％-5．3％，平均解吸效率为90％，采样效率为100％，样品在冷藏状态下（5℃）能保存10d。结论方法各项指标均符合GBZFF210．4-2008（职业卫生标准制定指南第4部分：工作场所空气中化学物质测定方法》的要求，适用于工作场所空气中蒸气态异氰酸甲酯的检测。

Objective To establish the method of detecting the concentrations of methyl isocyanate （MIC） in air ofworkplaces with high performance liquid chromatographic （HPLC）. Methods Samples are collected by XAD-7 tubes coated with l-（2-pyridyl） piperazine （1-2PP）. Samples are desorbed with acetonitrile （ACN） and analyzed by high performance liquid chromatography （HPLC） using a fluorescence detector. Results There was a linear relationship within the range of 0.01×10μg/ml, and the detection limit was 5.3×10-4μg/ml.The minimum detectable concentration was 0.01μg/ml, and the lowest detected concentration was 3.3×10-3 mg/m3. The relative standard deviation was 2.2%-5.3%. The average desorption efficiency was 90% and the sampling effieiencies were 100%. The samples could be stored for 10 days in cold storage condition. Conclusion The present method could meet with the requirements of Guide for establishing occupational health standards-Part 4 Determination methods of air chemicals in workplace and be feasible for determination of MIC in workplace air.