微波萃取-超高效液相法测定PM2.5中的16种多环芳烃的方法

Determination of 16 polycyclic aromatic hydrocarbons in PM2.5 by ultra performance liquid chromatography with microwave extraction

目的建立微波萃取PM2.5中的16种多环芳烃,超高效液相荧光-紫外检测PM2.5中多环芳烃的方法。方法取1/8滤膜剪碎于萃取管中,加入15 ml乙腈微波萃取30 min,定量浓缩至1.0 ml,以乙腈、水为流动相进行梯度洗脱,用超高效液相紫外和荧光检测器测定。结果16种多环芳烃在0.050μg/ml~2.00μg/ml内线性相关系数≥0.9997,检出限在0.004μg/ml~0.017μg/ml,相对标准偏差在1.2%~5.6%,方法的平均回收率为70.0%~95.0%。结论超高效液相对16种多环芳烃有较好的分离效果,微波萃取对PM2.5中16种多环芳烃的提取效果较好。本方法操作简单,适合大批量样品的分析。

Objective Microwave assisted extraction was developed for determining the concentrations of 16 polycyclic aromatic hydrocarbons in PM2.5 by ultra performance liquid chromatograph with UV-fluorescence detector(UPLC-UV).Methods One eighth of the filter membrane was cut into pieces in the extraction tube,and 15 ml acetonitrile was added for microwave extraction for 30 min.Then the membrane was quantitatively concentrated to 1.0 ml.The mobile phases of acetonitrile and water were used for gradient elution,and the determination was made by UPLC-UV and fluorescence detector.Results The linearly dependent coefficient of the 16 PAHs within the scope of 0.050μg/ml-2.00μg/ml was equal to and greater than 0.9997;the detection limits ranged from 0.004μg/ml to 0.017μg/ml.The relative standard deviations were within 1.2%-5.6%and the average recoveries were from 70.0%to 95.0%.Conclusion The method in this study can effectively determine the concentrations of PAHs in PM2.5 and is suitable for the analysis of large numbers of samples because of its simplicity.