Focant Jean-François, Sjödin Andreas, Patterson Donald G
Centers for Disease Control and Prevention, National Center for Environmental Health, Division of Laboratory Sciences, Organic Analytical Toxicology Branch, 4770 Buford Hwy NE, Mail Stop F-17, Atlanta, GA 30341, USA.
J Chromatogr A. 2004 Jun 25;1040(2):227-38. doi: 10.1016/j.chroma.2004.04.003.
The separation of the 209 polychlorinated biphenyl (PCB) congeners has been studied using comprehensive two-dimensional gas chromatography coupled to time-of-flight mass spectrometry (GC x GC-TOFMS). Four column combinations based on thermally stable phases, DB-1/HT-8, DB-XLB/HT-8, DB-XLB/BPX-50, and HT-8/BPX-50, have been investigated. The HT-8/BPX-50 set produced the best separation. The distribution of the 100 to 150 ms wide peaks was highly structured in the chromatographic space and based on the degree of ortho-substitution within each separated homologue series. A total of 192 congeners were resolved in 146 min (1.3 analyte per min) using this column set. Eight coelutions involved 17 congeners. Among them, seven congeners were present in Aroclors at levels >1.0 wt.% (CBs 33, 47, 48, 95, 97, 163, 187). Except for CBs 47 and 48, none of the major constituents of commercial mixtures were coeluting. CB 138 was well separated from CBs 163 and 164 in the second dimension. For all column sets, CBs 20, 33, and 109 always coeluted with other PCBs. The 12 toxic dioxin-like congeners (CBs 77, 81, 105, 114, 118, 123, 126, 156, 157, 167, 169, 189), and the seven European Union marker PCBs (CBs 28, 52, 101, 118, 138, 153, 180) were separated from any interfering congeners. This was not the case for the other investigated column sets.
采用全二维气相色谱-飞行时间质谱联用技术（GC×GC-TOFMS）对209种多氯联苯（PCB）同系物进行了分离研究。考察了基于热稳定固定相的四种柱组合，即DB-1/HT-8、DB-XLB/HT-8、DB-XLB/BPX-50和HT-8/BPX-50。HT-8/BPX-50柱组合分离效果最佳。在色谱空间中，100至150毫秒宽的峰分布具有高度的结构化，且基于每个分离的同系物系列中的邻位取代程度。使用该柱组合在146分钟内分离出了192种同系物（每分钟1.3种分析物）。有8处共流出涉及17种同系物。其中，7种同系物在多氯联苯混合物中的含量>1.0 wt.%（CBs 33、47、48、95、97、163、187）。除了CBs 47和48外，商业混合物的主要成分没有共流出的情况。CB 138在第二维中与CBs 163和164得到了很好的分离。对于所有柱组合，CBs 20、33和109总是与其他多氯联苯共流出。12种有毒的二噁英类同系物（CBs 77、81、105、114、118、123、126、156、157、167、169、189）以及7种欧盟标记多氯联苯（CBs 28、52、101、118、138、153、180）与任何干扰同系物实现了分离。其他考察的柱组合则并非如此。
