Analyses of Fish Tissue by Vacuum Distillation/Gas Chromatography/Mass Spectrometry

摘要

The analyses of fish tissue using VD/GC/MS with surrogate-based matrix corrections is described. Techniques for equilibrating surrogate and analyte spikes with a tissue matrix are presented, and equilibrated spiked samples are used to document method performance. The removal of analytes from the tissue corresponds to K↓(oa) and K↓(wa) (octanol-air and water-air partition coefficients, respectively). For a given vacuum distillation, the impact of K↓(oa) and K↓(wa) on analyte recovery can be determined by interpreting the recoveries of surrogate compounds and their K↓(oa) and K↓(wa). The use of these surrogates to monitor and correct for both water-air and octanol-air partitioning provides average recoveries of 86% for volatile gases, 97% for volatiles, 90% for neutral semivolatiles, 124% for basic semivolatiles, and 87% for the water-soluble volatiles. The method detection limits are sub-parts-per-billion for most analytes studied. A technique to experimentally determine the octanol-air partition relative volatility is described and the values for 113 compounds are presented.