气相色谱-质谱法同时测定饮用水中18种多氯联苯和16种多环芳烃

Simultaneous determination of 18 kinds of polychlorinated biphenyls and 16 kinds of polycyclic aromatic hydrocarbons in water by gas chromatography-mass spectrometry

目的建立一种利用固相萃取结合气相色谱-质谱法(GC-MS)同时检测饮用水中18种多氯联苯(polychlorinated biphenyls,PCBs)和16种多环芳烃(Polycyclic Aromatic Hydrocarbons,PAHs)残留的分析方法。方法水样加入5‰体积甲醇改良极性,使用固相萃取法提取,无水硫酸钠脱水,经旋转蒸发仪浓缩,采用TG-1701MS毛细管色谱柱,GC-MS进行分析,用外标法定量。结果在0.5μg/L~200.0μg/L的浓度范围内18种多氯联苯(PCBs)和16种多环芳烃(PAHs)能够有效分离、峰形较好,标准曲线线性关系良好,方法线性相关系数r>0.999,方法检出限为0.05 ng/L~3 ng/L,回收率为77.5%~124.5%,相对标准偏差(RSD)为0.84%~2.98%。结论该方法简便、快速、整体成本较低、实用性强,检测指标广,回收率和检出限均能满足样品分析质量控制要求,适合饮用水中多氯联苯(PCBs)和多环芳烃(PAHs)的同时检测分析。

Objective This paper aims to establish a method for the simultaneous detection of 18 polychlorinated biphenyls(PCBs)and 16 polycyclic aromatic hydrocarbons(PAHs)residues in drinking water by solid-phase extraction combined with gas chromatography-mass spectrometry(GC-MS).Methods The water samples were added with 5‰volume of methanol to improve the polarity.They are extracted by solid phase extraction,dehydrated with anhydrous sodium sulfate,and concentrated by rotary evaporator.TG-1701MS capillary column and GC-MS were adopted for analysis,and external standard method was used for quantification.Results The 18 polychlorinated biphenyls(PCBs)and 16 polycyclic aromatic hydrocarbons(PAHs)could be effectively separated in the concentration range of 0.5μg/L-200.0μg/L and showed good peak shape.The linearity of the standard curve was good.The linear correlation coefficient(r)of the method was more than 0.999.The detection limit of the method was within 0.05 ng/L-3 ng/L.The recoveries were within 77.5-124.5%.The relative standard deviations(RSDs)were within 0.84%-2.98%.Conclusion The method is convenient,rapid,practical and characterized by low cost and wide detection index.Recovery and detection limit meet the quality control requirements of sample analysis.It is suitable for the simultaneous detection and analysis of polychlorinated biphenyls(PCBs)and polycyclic aromatic hydrocarbons(PAHs)in drinking water.