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Analysis of estrogens in sediment from a sewage‐impacted urban estuary using high‐performance liquid chromatography/time‐of‐flight mass spectrometry
Author(s) -
Reddy Sharanya,
Brownawell Bruce J.
Publication year - 2005
Publication title -
environmental toxicology and chemistry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 1.1
H-Index - 171
eISSN - 1552-8618
pISSN - 0730-7268
DOI - 10.1897/04-167r.1
Subject(s) - mass spectrometry , chromatography , sediment , extraction (chemistry) , chemistry , matrix (chemical analysis) , wastewater , isotope dilution , solid phase extraction , environmental chemistry , high performance liquid chromatography , environmental science , geology , environmental engineering , paleontology
We describe a highly selective and sensitive method for determination of estrone (E1) and β‐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 E1 and E2, respectively) are sufficient to determine E1 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 E1 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 E1 and E2 ranged between 0.07 to 2.52 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.