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Quantitation of 17 α ‐ethinylestradiol in aquatic samples using liquid‐liquid phase extraction, dansyl derivatization, and liquid chromatography/positive electrospray tandem mass spectrometry
Author(s) -
Zhang Fagen,
Bartels Michael J.,
Brodeur Julie C.,
McClymont E. Lynn,
Woodburn Kent B.
Publication year - 2004
Publication title -
rapid communications in mass spectrometry
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.528
H-Index - 136
eISSN - 1097-0231
pISSN - 0951-4198
DOI - 10.1002/rcm.1690
Subject(s) - chemistry , chromatography , dansyl chloride , derivatization , electrospray , extraction (chemistry) , tandem mass spectrometry , liquid chromatography–mass spectrometry , detection limit , mass spectrometry , electrospray ionization , aqueous solution , solid phase extraction , high performance liquid chromatography , sample preparation , ethinylestradiol , population , demography , research methodology , sociology
A rapid and sensitive method for the analysis of 17 α ‐ethinylestradiol (EE 2 ) in environmental aqueous samples has been developed. Aquatic samples were extracted using liquid‐liquid extraction, and organic phase extracts were concentrated and derivatized with dansyl chloride. Analysis was performed using high‐performance liquid chromatography with positive electrospray ionization and tandem mass spectrometry (HPLC/ESI‐MS/MS). Deuterated 17 α ‐ethinylestradiol was used as internal standard and was added to samples before extraction. A limit of quantitation of 1 ng/L was obtained using a 25 mL aqueous sample. The average recovery of EE 2 spiked into a 25 mL tapwater sample was 100%. This highly sensitive quantitation method is useful for measuring low levels of EE 2 in aqueous environmental samples. Copyright © 2004 John Wiley & Sons, Ltd.