Analysis of estrogens in sediment from a sewage-impacted urban estuary using high-performace liquid chromatography/time-of-flight mass spectrometry
Reddy S and Brownawell BJ. 2005. Analysis of estrogens in sediment from a sewage-impacted urban estuary using high-performace liquid chromatography/time-of-flight mass spectrometry. Environmental Toxicology and Chemistry. 24(5):1041-1047
We describe a highly selective and sensitive method for determination ofestrone (El) and ^-estradiol (E2) in sediments, using high-performance liquid chromatography/time-of-flight (HPLC-ToF) mass spectrometry. The method involved sequential cleanup of sediment extracts over solid phase extraction cartridges, normal phase HPLC, and immunoaffinity extraction, which combine to remove coeluting matrix interferences. Resulting method detection limits (0.03 and 0.04 ng/g for El and E2, respectively) are sufficient to determine El and E2 in estuarine sediments collected from sewage-impacted Jamaica Bay (New York, NY, USA). The ToF analyzer has a higher resolution (>6,000) than quadrupole mass analyzers and can provide accurate mass estimation to within 2 mDa, which helped in distinguishing steroids from isobaric matrix interferences. The El and E2 were internally mass calibrated with respect to their coeluting surrogate standards, and the mass measurement error was between 1.1 and 1.4 mDa. The levels of El and E2 ranged between 0.07 to 2.S2 and 0.05 to 0.53 ng/g, respectively. The measured concentrations of steroids in sediments correlated closely with other wastewater tracers. Despite the low concentrations of sediment-associated estrogens, their predicted estrogenic potency exceeds that of other measured estrogenic contaminants.
- Type
- Journal Article
- Authors
- Reddy, Sharanya; Brownawell, Bruce
- Units
- GATE
- Keywords
- estrogens, High-performance liquid chromatography, Mass spectrometry, Sediments, steroids