Determination of alkylphenol and alkylphenolethoxylates in biota by liquid chromatography with detection by tandem mass spectrometry and fluorescence spectroscopy
Résumé
A quantitative method for the simultaneous determination of octylphenol, nonylphenol and the corresponding ethoxylates
(1 to 5) in biota is presented. Extraction methods were developed for egg and fish matrices based on accelerated solvent
extraction followed by a solid-phase extraction cleanup, using octadecylsilica or aminopropyl cartridges. Identification and
quantitation were accomplished by liquid chromatography–electrospray tandem mass spectrometry (LC–MS–MS) and
compared to the traditional liquid chromatography with fluorescence spectroscopy detection. LC–MS–MS provides high
13 sensitivity and specificity required for these complex matrices and an accurate quantitation with the use of C-labeled
internal standards. Quantitation limits by LC–MS–MS ranged from 4 to 12 ng/g in eggs, and from 6 to 22 ng/g in fish
samples. These methods were successfully applied to osprey eggs from the Chesapeake Bay and fish from the Great Lakes
area. Total levels found in osprey egg samples were up to 18 ng/g wet mass and as high as 8.2 mg/g wet mass in the fish
samples.