Analysis of C-14-C-17 polychloro-n-alkanes in environmental matrixes by accelerated solvent extraction-nigh-resolution gas chromatography/electron capture negative ion high-resolution mass spectrometry

A method for quantifying medium-chain (C-14-C-17) polychloroalkanes (mPCAs) in environmental matrixes by accelerated solvent extraction high-resolutio n gas chromatography/electron capture negative ion high-resolution mass spe ctrometry in the selected ion monitoring mode is presented. The formula gro up abundance profiles of industrial mPCA mixtures, which are used as standa rds, and of samples are first determined by monitoring [M-Cl](-) ions of sp ecific m/z values corresponding to the molecular formulas present and by co rrecting the integrated ion signals for the fractional abundance of the spe cific m/z value monitored and the number of chlorine atoms in the formula g roup. mPCA concentrations in environmental samples are then determined by c omparing the response of a specific m/z peak in the sample to that in the s tandard. Extraction recoveries of mPCAs from spiked fish and sodium sulfate tin place of sediment) were >79%. Method detection limits were 13 ng/g for fish and 1.4 ng/mu L for sediment, while the analytical detection limit wa s similar to 200 pg, at a signal-to-noise ratio of 4:1. By this method, mPC As were detected in biota and sediment from the mouth of the Detroit River (MI) and ranged from 70 to 900 ng/g, The simultaneous quantitation of C-10- C-13 (sPCAs) and C-14-C-17 PCAs, based on monitoring two specific m/z peaks , one characteristic of sPCAs and the other of mPCAs, is also demonstrated.