Rapid determination of free and conjugated estrogen in different water matrices by liquid chromatography-tandem mass spectrometry

Kumar, Vimal; Nakada, Norihide; Yasojima, Makoto; Yamashita, Naoyuki; Johnson, Andrew C.; Tanaka, Hiroaki. 2009 Rapid determination of free and conjugated estrogen in different water matrices by liquid chromatography-tandem mass spectrometry. Chemosphere, 77 (10). 1440-1446.

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This article describes the development of a short pre-treatment method that allows the simultaneous analysis of free estrogens (estrone, 17β-estradiol, estriol and 17-ethynylestradiol) and their sulphate and glucuronide conjugated forms. For a range of matrices, from sewage effluent to river water, the developed methodology based on solid phase extraction and fractionation technique with ultra-performance liquid chromatography system showed effective separation of the targeted estrogens. The detection limits of this method ranged from 0.2 to 0.8 ng L–1 for river water. The recoveries for river water and sewage effluent varied from 63 to 127%. The problems of matrix effects and ion suppression, or enhancement, were allowed quantitatively for in the analysis using standard addition. The developed method was used successfully to detect estrogens and their conjugates in both raw and treated wastewater, and river water at a location in Japan. High concentrations of the free estrogens estrone, 17β-estradiol and estriol were found in the influent (22.6, 77.2, 64.6 ng L–1 respectively) but only E1 was still present at a high concentration in the effluent which was reflected in the downstream river concentration. Estrone-3-sulphate was detected up to 18.0 ng L–1 in influent water sample and 1.1 ng L–1 in downstream water. For the sulphate conjugates, removal efficiencies varied from 35 to 88%.. Glucuronide conjugates were detected only once in the sewage influent.

Item Type: Publication - Article
Digital Object Identifier (DOI):
Programmes: CEH Programmes pre-2009 publications > Water > WA02 Quantifying processes that link water quality and quantity, biota and physical environment > WA02.2 Hydrochemical and sediment processes
UKCEH and CEH Sections/Science Areas: Acreman
ISSN: 0045-6535
Additional Keywords: short pre-treatment, free and conjugated estrogen, UPLC/MS/MS, matrix effect
NORA Subject Terms: Ecology and Environment
Date made live: 01 Apr 2010 12:50 +0 (UTC)

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