雾霾PM2.5中7种指示性多氯联苯的微波辅助萃取气相色谱三重四极杆串联质谱法

Determination of 7 indicator polychlorinated biphenyls in fog PM2.5 by microwave-assisted extraction coupled with gas chromatography-triple quadrupole mass spectrometry

目的建立雾霾PM2.5中痕量7种指示性多氯联苯的微波辅助萃取气相色谱三重四极杆串联质谱(GC-MS/MS)检测方法。方法采样后的雾霾PM2.5玻璃纤维滤膜经微波辅助萃取,佛罗里硅土柱净化后,用GC-MS/MS测定。结果 7种指示性多氯联苯在0.5~100μg/L范围内线性良好,线性回归系数r≥0.999,仪器检出限为0.03~0.06μg/L,方法检出限为0.042~0.084 pg/m^3,加标回收率为74.5%~94.5%,相对标准偏差RSD(n=6)为2.1%~3.6%。结论该方法灵敏、准确,有效去除了基质干扰,适用于雾霾PM2.5中7种指示性多氯联苯的测定。

Objective To develop a new method for the rapid determination of trace seven kinds of indicator polychlorinated biphenyls（ PCBs） in fog PM2.5 by using Microwave- assisted extraction（ MAE） coupled with gas chromatography- triple quadruple mass spectrometry（ GC- MS / MS）. Methods The particle samples of fog PM2.5 was collected by high- volume active sampling devices on glass fiber filter in Shijiazhuang City,seven congeners of PCBs were extracted by Microwave- assisted extraction（MAE）,and cleaned up with Florisil solid phase extraction（SPE） column. The analysis of PCBs was performed with GC- MS/MS. Results The linear regression coefficients of the seven PCBs were in the range of 0. 5 ～ 100 μg / L. The linear regression coefficients were over 0. 9 999 and the detection limits were 0. 03 ～ 0. 06 μg / L. The detection limit was 0. 042 ～ 0. 084 pg / m^3,and the relative standard deviations RSD（ n = 6） ranged from 2. 1% to 3. 6% with the recoveries of 74. 5% ～ 94. 5%. Conclusion After the exclusion of matrix interference,this method was green,fast,simple,sensitive and accurate,applicable to determination of seven kinds of indicator PCBs in fog PM2.5.