大气PM2.5中18种多氯联苯的超声提取-气相色谱-高分辨质谱联用测定法

Determination of 18 polychlorinated biphenyls in PM2.5 by ultrasonic extraction-gas chromatography-high resolution mass spectrometry

目的建立大气PM2.5中18种多氯联苯(PCBs)的超声提取-气相色谱-高分辨质谱(GC-HRMS)联用测定法。方法采样滤膜经超声提取、层析柱净化、氮吹浓缩后,采用GC-HRMS法进样分析。结果18种PCBs在0.015~5.00 pg/m3的范围内,所得回归方程均呈良好的线性关系(r≥0.997)。方法的检出限为0.009~0.018 pg/m3,定量下限为0.028~0.055 pg/m3,平均回收率为76.0%~122.0%,RSD为2.3%~18.1%。结论该方法操作简单、灵敏度高、选择性强,适用于大气PM2.5中18种PCBs的同时测定。

Objective To develop a method for the simultaneous determination of 18 polychlorinated biphenyls(PCBs)in PM2.5 by ultrasonic extraction-gas chromatography-high resolution mass spectrometry(GC-HRMS).Methods The sample filter membrane was extracted by ultrasonic method,cleaned by chromatographic column,the eluate was concentrated with nitrogen and detected with gas chromatography-high resolution mass spectrometry(GC-HRMS).Results The calibration curves of 18 polychlorinated biphenyls showed a good linearity in the range of 0.015-5.00 pg/m3 respectively,and the correlation coefficients were more than 0.997.The limits of detection were 0.009-0.018 pg/m3,the limits of quantification were 0.028-0.055 pg/m3.The spiked recoveries ranged from 76.0%to 122.0%and the relative standard deviations ranged from 2.3%to 18.1%.Conclusion This method is easy,accurate,sensitive and applicable to the determination of 18 polychlorinated biphenyls(PCBs)in PM2.5.