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目的建立大气PM_(2.5)中20种指示性多氯联苯的加速溶剂萃取-气相色谱三重四极杆质谱法。方法样品经加速溶剂萃取、减压浓缩、佛罗里硅土柱净化、洗脱液浓缩后,用气相色谱三重四级杆质谱多重反应监测模式检测,以外标法定量。结果 20种多氯联苯在0.5~100μg/L范围内线性良好,相关系数(r值)≥0.999,仪器检出限为0.03~0.34μg/L,方法检出限为0.045~0.50 pg/m~3。加标回收率除三氯联苯(PCB18)为74.4%外,其余均在89.4%~119.8%之间;相对标准偏差(RSD)<5%。结论该方法提取时间短、溶剂用量少、灵敏可靠、成本低廉,适用于大气PM_(2.5)中20种指示性多氯联苯的快速检测。
Objective To establish an accelerated solvent extraction - gas chromatography triple quadrupole mass spectrometry for the determination of 20 indicative polychlorinated biphenyls in PM 2.5 atmosphere. Methods The samples were extracted by accelerated solvent extraction and concentrated under reduced pressure. The Florisil silica column was purified and the eluent was concentrated. The samples were detected by gas chromatography triple quadrupole mass spectrometry multiplex reaction monitoring mode and quantified by external standard method. Results The linearities of 20 PCBs in the range of 0.5-100 μg / L were good with the correlation coefficient (r value) ≥0.999, detection limit of 0.03 ~ 0.34 μg / L and detection limit of 0.045 ~ 0.50 pg / m ~ 3. The spiked recoveries were all within the range of 89.4% -119.8% with the PCB18 of 74.4%. The relative standard deviations (RSDs) were less than 5%. Conclusion The method has the advantages of short extraction time, less solvent usage, high sensitivity and low cost, and is suitable for the rapid detection of 20 indicative polychlorinated biphenyls in atmospheric PM_ (2.5).