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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-triazol-5-one in workplace air by high performance liquid chromatography. Methods: ODSC18 column (200 mm × 4.6 mm × 5 μm) was used. The mobile phase was water: glacial acetic acid: triethylamine = 800: 2:1. The flow rate was 1.0 ml / min. The detection wavelength was 220 nm. Results: The limit of detection was 0.30 μg / mL (injection of 10 μl of eluent) with a minimum detectable concentration of 0.004 mg / m3 for 150 L air samples. The regression equation was y = 26.51x-4.06 with a correlation coefficient of r = 0.9999. The relative standard deviations (RSDs) were 1.0% -1.1% and the elution efficiencies were 98.3% -99.7% for the samples with high, medium and low concentrations. The recoveries ranged from 96.9% to 102.2%. Samples were stored for at least 14 days at room temperature. Under this condition, trinitrotoluene could coexist with 3-nitro-1,2,4-triazol-5- Today, Akito did not interfere with this determination. Conclusion: The method has the advantages of simple sample processing, short determination period, high sensitivity and good reproducibility. It is suitable for the detection of 3-nitro-1,2,4-triazol-5-one in the air of workplace.