Determination of Estrogens in Sludge and Sediments by Liquid Extraction and GC/MS/MS

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Abstract
Two methods have been developed that enable the determination of estrogens down to 2 ng/g in digested and activated sludge from domestic sewage treatment plants (STPs) and down to 0.2 ng/g in freshwater sediments. The method for sludge analysis consists of solvent extraction; a gel permeation chromatography (GPC) cleanup step, a 1 g silica gel column; and finally, detection by GC-ion trap MS/MS of the silylated estrogens with MSTFA. For sediments, the solvent extraction was successively followed by silica gel cleanup, solid phase enrichment (SPE), and a HPLC cleanup before derivatization and GC/MS/MS detection. Mean recoveries of the estrogens mainly exceeded 70% in sludge and 90% in sediments. In activated and digested sewage sludge, estrone and 17beta-estradiol were detected up to 37 ng/g and 49 ng/g, respectively, and 17alpha-ethinylestradiol up to 17 ng/g. The occurrence of estrogens in digested sludge indicates that estrogens can be persistent during sludge digestion. In river sediments, estrone and 17beta-estradiol were detected up to 2 ng/g (estrone), and the contraceptive 17alpha-ethinylestradiol was found with a maximum of 0.9 ng/g. Mestranol, a prodrug for 17alpha-ethinylestradiol, was not detected either in sludge or in sediments.

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