工作场所空气中3-硝基-1,2,4-三唑-5-酮的高效液相色谱测定方法

Determination of 3-nitro-1,2,4-tirzol-5-one in workplace air by high performance liquid chromatography

目的:建立工作场所空气中3-硝基-1,2,4-三唑-5-酮的高效液相色谱测定方法。方法:采用ODSC18柱(200 mm×4.6 mm×5μm);流动相∶水∶冰乙酸∶三乙胺=800∶2∶1;流速:1.0 ml/min;检测波长:220 nm。结果:检出限为0.30μg/mL(进样10μl洗脱液),最低检出浓度为0.004 mg/m3(以采集150 L空气样品计)。回归方程为y=26.51x-4.06,相关系数为r=0.9999,高、中、低三个浓度的样品,相对标准偏差为1.0%～1.1%,洗脱效率为98.3%～99.7%,方法的回收率为96.9%～102.2%,样品在室温至少可保存14 d,在该条件下与3-硝基-1,2,4-三唑-5-酮可能共存的三硝基甲苯、黑索今、奥克托今等不干扰测定。结论:该方法具有样品处理简便、测定周期短、灵敏度高、重现性好的优点,适用于工作场所空气中3-硝基-1,2,4-三唑-5-酮的检测。

Objective：To establish a method for the determination of 3-Nitro-1,2,4-tirzol-5-one in workplace air by high performance liquid chromatography.Methods： HPLC was carried ouf in the ODSC18 pillars（200 mm×4.6 mm×5 μm）with water-aceticacid-triethylamine（800∶2∶1）as a mobile phase of current velocity 1.0 ml/min,the detective wavelength was 220 nm.Results： The limit of the method was 0.30 μg/ml（resent 10 μl eluent）.The lowest concentration limit was 0.004 mg/m3（acquisit 150 L air for test sample）.Icariin regression equation was y=26.51x-4.06（r=0.9999）.Determine high hit and low concentration sample,the relative standard deviation was 1.0%～1.1%,the elution efficiency was 98.3%～99.7% and the percent recovery was96.9%～102.2%.The samples could be stored for at least 14days at room temperature.Trinitrotolucne,Cydonite,Octogen which may coexist with 3-Nitro-1,2,4-tirzol-5-one were not the interfering factor.Conclusion： HPLC detection methods has the characteristics of simple sample handling,rapid determination,high sensitivity and good reproducibility,it could be used for determining 3-Nitro-1,2,4-tirzol-5-one and detect sample purity in workplace air.