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Analysis of estrogenic contaminants in river water using liquid chromatography coupled to ion trap based mass spectrometry
Author(s) -
Benijts Tom,
Dams Riet,
Günther Wolfgang,
Lambert Willy,
Leenheer André De
Publication year - 2002
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.716
Subject(s) - chemistry , chromatography , detection limit , mass spectrometry , ion trap , estriol , sample preparation , solid phase extraction , solvent , extraction (chemistry) , analytical chemistry (journal) , biochemistry , organic chemistry , hormone
A precise and reliable method, using liquid chromatography combined with ion trap based mass spectrometry, for the determination of three endogenous estrogens, namely, estrone, estradiol, and estriol, and two synthetic estrogens, ethinyl estradiol and diethylstilbestrol, in environmental water samples was developed. Optimization of the parameter settings of the ion source and mass analyzer as well as evaluation of solvent composition were carried out by continuous introduction of standards through a syringe pump. In negative ion mode the electrospray ionization source gave acceptable results. The optimum solvent used consisted of water/acetonitrile, with no volatile bases or buffers added. A simple, off‐line, manual solid‐phase extraction method was developed for sample preparation of environmental water samples. Recoveries were over 86% for all compounds. The method was validated and found to be linear, selective, and robust. For analysis of a 50‐mL sample, the limit of detection (LOD) ranged from 3.2 to 10.6 ng/L for all compounds, and the limit of quantitation (LOQ) from 10.6 to 35.0 ng/L. Within‐day (n = 5) and total (n = 5) reproducibility were investigated at three different concentration levels and ranged from 6.2 to 9.5% and 9.4 to 12.1%, respectively. Finally, the method was applied to real‐world samples. Copyright © 2002 John Wiley & Sons, Ltd.