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目的建立工作场所空气中苯醌的液相色谱检测方法。方法空气中的苯醌用溶剂解吸型硅胶管采集,乙腈解吸,经液相色谱柱(XDB-C18)分离,DAD检测器检测,以保留时间定性,峰面积定量。结果方法的测定范围为0.5μg/ml~25μg/ml,检出限为0.05μg/ml,定量下限为0.15μg/ml,批内精密度为2.32%~3.59%,批间精密度为1.84%~5.47%,方法的加标回收率为99%~107%,本法平均采样效率为100%,解吸效率为96.1%~99.5%,硅胶管采集苯醌后室温可保存14 d。结论方法的检出限、精密度、加标回收率、采样效率、解析效率、样品稳定性符合《工作场所空气中有毒物质检测方法研制规范》的要求,适用于工作场所空气中苯醌浓度的测定。
Objective To establish a method for the determination of benzoquinone in the air of the workplace by liquid chromatography. Methods The benzoquinone in air was collected by desorption type silica gel tube, desorbed by acetonitrile, separated by liquid chromatography column (XDB-C18) and detected by DAD detector. The retention time was qualitative and the peak area was quantified. Results The determination range was 0.5μg / ml ~ 25μg / ml, the detection limit was 0.05μg / ml, the limit of quantitation was 0.15μg / ml, the intra-assay precision was 2.32% ~ 3.59%, the inter- ~ 5.47%. The spiked recoveries were 99% -107%. The average sampling efficiency was 100% and the desorption efficiency was 96.1% ~ 99.5%. The silica gel tube was stored at room temperature for 14 days after benzoquinone extraction. Conclusions The detection limits, precision, spike recovery, sampling efficiency, analytical efficiency and sample stability are in accordance with the requirements of the “Norms for the Development of Test Methods for Toxic Substances in the Air at Work”, and are suitable for the concentration of benzoquinone in the air of the workplace Determination.