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Simultaneous separation of coplanar and chiral polychlorinated biphenyls by off-line pyrenyl-silica liquid chromatography and gas chromatography. Enantiomeric ratios of chiral congeners

机译:离线pyr-硅胶液相色谱和气相色谱法同时分离共平面和手性多氯联苯。手性同类物的对映体比率

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摘要

A method for the unambiguous determination of 41 key polychlorinated biphenyls (PCBs) (including coplanar and chiral congeners) and the enantiomeric ratio of chiral congeners is described. The method includes a fractionation step using a 2-(1-pyrenyl) ethyldimethylsilylated silica column for separating the polychlorinated biphenyls according to the number of chlorine atoms in the ortho positions. High-resolution gas chromatography with an electron capture detector and an achiral column was used to determine the PCB congener content in each fraction. The enantiomeric ratio of chiral congeners was calculated by high-resolution gas chromatography with a mass spectrometry detector using a chiral column. The method was found to be inexpensive, rapid, effective, and reliable under the operational conditions proposed, It eliminates the main coelution problems among the polychlorinated biphenyl congeners, It also makes it possible to determine the enantiomeric ratio of nine chiral congeners using monodimensional gas chromatography. The method was applied successfully to the analysis of the coplanar and atropisomeric polychlorinated biphenyl congeners in dolphin liver samples. The enantiomeric ratio of nine chiral congeners is also reported for the first time. [References: 49]
机译:描述了一种确定41种关键多氯联苯(PCBs)(包括共平面和手性同类物)和手性同类物对映体比例的方法。该方法包括使用2-(1-吡啶基)乙基二甲基甲硅烷基化的二氧化硅柱的分馏步骤,以根据邻位上的氯原子数分离多氯联苯。带有电子捕获检测器和非手性色谱柱的高分辨率气相色谱法用于确定每个馏分中的PCB同类物含量。手性同源物的对映体比率是通过使用手性柱的质谱检测器通过高分辨率气相色谱来计算的。在所提出的操作条件下,该方法廉价,快速,有效,可靠,消除了多氯联苯同源物之间的主要共洗脱问题,也使使用一维气相色谱法测定九种手性同源物的对映体比率成为可能。 。该方法已成功地用于分析海豚肝样品中的共面和阻转异构的多氯联苯同源物。还首次报道了九种手性同源物的对映体比率。 [参考:49]

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