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Determination of estrogenic steroids in surface water and wastewater by liquid chromatography–electrospray tandem mass spectrometry
Author(s) -
Zuehlke Sebastian,
Duennbier Uwe,
Heberer Thomas
Publication year - 2005
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200301727
Subject(s) - chemistry , chromatography , wastewater , surface water , effluent , solid phase extraction , tandem mass spectrometry , mass spectrometry , electrospray ionization , liquid chromatography–mass spectrometry , detection limit , sewage treatment , matrix (chemical analysis) , extraction (chemistry) , sewage , electrospray , analyte , environmental chemistry , environmental engineering , environmental science
An analytical method is presented which permits trace level determination of 17α‐ethynylestradiol (EE2), 17β‐estradiol (E2), and estrone (E1). Using this method, the estrogenic steroids were analyzed in drinking water, surface water, and wastewater (sewage influents and effluents) at concentrations down to 0.1 ng/L. Sample volumes between 100 and 500 mL are concentrated using automated solid‐phase extraction. Analysis is performed by liquid chromatography with detection by tandem mass spectrometry. Applying simple clean‐up procedures and internal standard calibration, recovery losses resulting from matrix‐dependent ion suppression during electrospray ionization could be compensated for all of the investigated compounds. Recoveries around 100% were obtained for all analytes after correction using the internal standards. Limits of quantification (LOQ) were between 0.1 and 0.4 ng/L for purified sewage, surface, ground, and drinking water and between 1 and 2 ng/L in the case of raw sewage. Water treatment by wastewater treatment plants (WWTPs) or by a surface water treatment plant affected the removal of all estrogenic steroids. Thus, E1, E2, and EE2 were removed in the municipal WWTPs to the extent of 93%, 93%, and 80%, respectively. In the effluents of the WWTP in Ruhleben (Berlin, Germany), E1, E2, and EE2 were detected at the low ng/L level. E2 and EE2 were, however, not present in the Berlin surface water above the LOQ (0.2 ng/L). E1 was the only compound that could be detected in surface water samples. After additional surface water treatment it was still detectable but only at trace‐level concentrations with a mean value of 0.16 ng/L.