工作场所空气中苯醌测定方法的研究

Study on the method in determining benzoquinone in the air of workplace

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 high performance liquid chromatography（ HPLC） method for the determination of benzoquinone in the air of workplace. Methods Benzoquinone in workplaces air samples were collected with solvent desorption silica gel tube and desorbed with acetonitrile,and then separated with HPLP columns（ XDB-C18）; the samples were determined with DAD detector in order to retain the qualitative time and the quantitative area. Results The linear ranges of this method was0. 5 μg / ml-25 μg / ml,and the detection limit of this method was 0. 05 μg / ml,the quantitative limit was 0. 15 μg / ml. The within-batch precision of this method was within 2. 32%-3. 59%,the between-run precision was within 1. 84%-5. 47%,and the recovery rate was within 99%-107%. The average sampling efficiency and the desorption rate of this method were100% and within 96. 1%-99. 5%,respectively. The benzoquinone sampled with solvent desorption silica gel tube could at least stored for 14 days at room temperature. Conclusion The detection limit,recovery rate,sampling efficiency,desorption rate,precision and sample stability of this method meet the requirement of Specification for the Development of Detection Methods for Toxic Substances in the Air of Workplace,which is suitable for the determination of benzoquinone in the air of workplaces.