Coupled LC‐GC‐MS for on‐line clean‐up, separation, and identification of chlorinated polycyclic aromatic hydrocarbons at picogram levels in urban air

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Abstract
Coupled liquid chromatography – gas chromatography – mass spectrometry (LC‐GC‐MS) has been applied for on‐line clean up, separation, and identification of chlorinated polycyclic aromatic hydrocarbons (CI‐PAHs). A loop‐type interface was used to couple the liquid chromatograph on‐line with the GC‐MS, and concurrent solvent evaporation was used for sample transfer.A back‐flush technique was used in conjunction with a two‐dimensional column system for isolation of CI‐PAHs and polycyclic aromatic hydrocarbons (PAHs). This fraction was transferred on‐line to the GC and separated on a capillary column. Selective and sensitive detection of CI‐PAHs in the GC eluate was obtained by negative ion chemical ionization (NICI) mass spectrometry and selected ion monitoring (SIM).The combined on‐line system for isolation, separation, and identification showed high precision and accuracy, and demonstrated a linear response from 1 to 1000 pg for chlorinated PAHs. The estimated detection limit was 250 fg for 1‐chloropyrene and 1,6‐dichloropyrene.The technique was demonstrated by analysis of urban air samples. The low detection limit made it possible to use the technique for analysis of personally carried monitoring equipment for measurement of exposure to CI‐PAHs in the work environment.

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