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(03-04) Analysis of estrogens and progestogens in sewage sludge by liquid chromatography/mass spectrometry. Barceló, Damiŕ1, López, Ramón1, López de Alda, Maria*,1, 1 Institute of Environmental and Chemical Research (IIQAB-CSIC), Barcelona, Spain ABSTRACT- In this study, an analytical procedure for the determination in sewage sludge of the most abundant and/or physiological active estrogens, both free (estradiol, estriol, estrone, ethynyl estradiol, and diethylstilbestrol) and conjugated (estradiol glucuronide, estrone, sulphate, estradiol acetate), and progestogens (progesterone, norethindrone, and levonorgestrel) is described. The procedure includes ultrasonic extraction of the lyophilized sewage sludge, clean-up with octadecylsilica and amino cartridges in series, and analysis by liquid chromatography-diode array detection-mass spectrometry (LC-DAD-MS). Chromatographic separation is carried out on a LiChrospher 100 RP-18 column (250×4 mm, 5 Key words: estrogens, sewage sludge , endocrine disrupters, analysis |
m) with gradient acetonitrile/water as mobile phase. MS detection is performed with an electrospray interface in the positive ion mode for determination of progestogens and in the negative ion mode for determination of estrogens. Detection limits varied between 20 and 500 ng/g. The method was applied to the determination of the target compounds in sewage sludge samples from the area of Catalonia (N.E. Spain). To the authors' knowledge, this is the first work reporting a detailed method for the environmental analysis of estrogens and/or progestogens in sewage sludge and data on their occurrence. Acknowledgements This work has been supported by the Energy, Environmental and Sustainable Development (EESD) Program (Project AWACSS EUK1-CT-2000-00045), and by the Ministerio de Ciencia y Tecnología (Project PPQ 2000-3006-CE). Merck (Darmstadt, Germany) is acknowledged for the gift of LC columns.