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ANALYTICAL METHODS AND QUALITY ASSURANCE CRITERIA FOR LC/ES/MS DETERMINATION OF PFOS IN FISH
Citation:
Kuehl, D W. ANALYTICAL METHODS AND QUALITY ASSURANCE CRITERIA FOR LC/ES/MS DETERMINATION OF PFOS IN FISH. Presented at American Society for Mass Spectrometry, Montreal, Quebec, Canada, June 8-12, 2003.
Description:
PFOS, perfluorooctanesulfonate, has recently received much attention from environmental researchers. Previous analytical methods were based upon complexing with a strong ion-pairing reagent and extraction into MTBE. Detection was done on a concentrate using negative ion LC/ES/MS/MS. Our attempts to use this method resulted in irreproducible data and low recoveries. Ion suppression, a phenomenon to which ES is susceptible, was thought to be at least partially responsible for these results when it was shown that the signal for PFOS (mz/499) was increasingly suppressed by the addition of an extract of control fish liver. Therefore, we developed an alternate method to obtain an extract that did not cause suppression of PFOS, and which could be done by MS rather than MS/MS. - - - PFOS in fish nearing steady state (12 h after dose) distributed nearly equal to serum and liver, with eggs and muscle at 10% and 1% of the liver values, respectively. A survey of Great Lakes trout liver (2 fish/lake) showed 5-250 ppb concentrations of PFOS.