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首页> 外文期刊>Analytical and bioanalytical chemistry >Automated clean-up, separation and detection of polycyclic aromatic hydrocarbons in particulate matter extracts from urban dust and diesel standard reference materials using a 2D-LC/2D-GC system
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Automated clean-up, separation and detection of polycyclic aromatic hydrocarbons in particulate matter extracts from urban dust and diesel standard reference materials using a 2D-LC/2D-GC system

机译：使用2D-LC / 2D-GC系统自动净化，分离和检测城市灰尘和柴油标准参考物质中颗粒物提取物中的多环芳烃

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A multidimensional, on-line coupled liquid chromatographic/gas chromatographic system was developed for the quantification of polycyclic aromatic hydrocarbons (PAHs). A two-dimensional liquid chromatographic system (2D-liquid chromatography (LC)), with three columns having different selectivities, was connected on-line to a two-dimensional gas chromatographic system (2D-gas chromatography (GC)). Samples were cleaned up by combining normal elution and column back-flush of the LC columns to selectively remove matrix constituents and isolate well-defined, PAH enriched fractions. Using this system, the sequential removal of polar, mono/diaromatic, olefinic and alkane compounds from crude extracts was achieved. The LC/GC coupling was performed using a fused silica transfer line into a programmable temperature vaporizer (PTV) GC injector. Using the PTV in the solvent vent mode, excess solvent was removed and the enriched PAH sample extract was injected into the GC. The 2D-GC setup consisted of two capillary columns with different stationary phase selectivities. Heart-cutting of selected PAH compounds in the first GC column (first dimension) and transfer of these to the second GC column (second dimension) increased the baseline resolutions of closely eluting PAHs. The on-line system was validated using the standard reference materials SRM 1649a (urban dust) and SRM 1975 (diesel particulate extract). The PAH concentrations measured were comparable to the certified values and the fully automated LC/GC system performed the clean-up, separation and detection of PAHs in 16 extracts in less than 24 h. The multidimensional, on-line 2D-LC/2D-GC system eliminated manual handling of the sample extracts and minimised the risk of sample loss and contamination, while increasing accuracy and precision. [Figure not available: see fulltext.]
机译：开发了一种多维在线耦合液相色谱/气相色谱系统，用于定量多环芳烃（PAH）。具有三个具有不同选择性的色谱柱的二维液相色谱系统（二维液相色谱（LC））在线连接到二维气相色谱系统（二维气相色谱（GC））。通过将常规洗脱和LC色谱柱的柱反吹相结合，可以选择性地去除基质成分并分离出定义明确的，富含PAH的馏分，从而净化了样品。使用该系统，可以从粗提物中依次除去极性，单/二价，烯烃和烷烃化合物。使用熔融二氧化硅传输线将LC / GC耦合到可编程温度蒸发器（PTV）GC进样器中。在溶剂排放模式下使用PTV，可以去除过量的溶剂，然后将富集的PAH样品萃取液注入GC。 2D-GC设置由两个具有不同固定相选择性的毛细管柱组成。在第一个GC色谱柱（第一维）中对选定的PAH化合物进行心脏切割并将其转移到第二个GC色谱柱（第二维）中，可以提高紧密洗脱的PAH的基线分离度。在线系统已使用标准参考材料SRM 1649a（城市尘土）和SRM 1975（柴油颗粒提取物）进行了验证。测得的PAH浓度与认证值相当，全自动LC / GC系统在不到24小时的时间内完成了16种提取物中PAH的净化，分离和检测。多维在线2D-LC / 2D-GC系统消除了对样品提取物的人工处理，并最大程度降低了样品丢失和污染的风险，同时提高了准确性和精度。 [图不可用：请参见全文。]

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