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采用同位素内标稀释-高分辨气相色谱-高分辨质谱法同时测定土壤及沉积物样品中PCDD/Fs、PBDD/Fs、DL-PCBs和PBDEs 4种二英类持久性有机物的含量.利用凝胶渗透色谱、多层酸碱硅胶净化柱、活性炭分散硅胶净化柱针对不同二英类污染物的不同吸附特性,运用不同极性的溶剂淋洗,实现二英组分(PCDD/Fs、PBDD/Fs)和其他两个组分(DL-PCBs、PBDEs)的分离,排除了同系物间及其他物质的干扰.所建方法的精密度变化范围在1.4%—13.6%之间,净化内标回收率范围在61%—104%之间,PCDD/Fs和PBDD/Fs的检出限分别在0.048—0.153 pg·g-1和0.044—0.395 pg·g-1之间,DL-PCBs和PBDEs的检出限分别在0.028—0.105 pg·g-1和0.034—10.2 pg·g-1之间,目标物检测结果大部分在质控样品标准范围之内,本文所建立的方法可以用于土壤及沉积物中PCDD/Fs、PBDD/Fs、DL-PCBs和PBDEs的同时净化分离.
Simultaneous determination of four dioxin-type persistent organic compounds (PCDD / Fs, PBDD / Fs, DL-PCBs and PBDEs) in soil and sediment samples by isotope dilution-high resolution gas chromatography-high resolution mass spectrometry Permeation chromatography, multi-layer acid-base silica gel purification column and activated carbon dispersion silica gel column were used to achieve different adsorption characteristics of different dioxin-like pollutants. The two components (PCDD / Fs, PBDD / Fs ) And other two components (DL-PCBs, PBDEs), excluding the interference between homologues and other substances.The precision of the proposed method ranged from 1.4% to 13.6%, and the internal standard recovery The detection limits of PCDD / Fs and PBDD / Fs were between 0.048-0.153 pg · g-1 and 0.044-0.395 pg · g-1, respectively. The detection limits of DL-PCBs and PBDEs ranged from 61% to 104% The limits of detection were between 0.028-0.105 pg · g-1 and 0.034-10.2 pg · g-1, respectively. Most of the detection results were within the standard range of the control sample. The method established in this paper can be applied to soil and sediment Simultaneous purification and separation of PCDD / Fs, PBDD / Fs, DL-PCBs and PBDEs.