PubMed · 13621915
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J F LALLY, W A REED. 1959. Genitourinary bleeding.. https://pubmed.ncbi.nlm.nih.gov/13621915/
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A procedure for the determination of six natural and synthetic estrogens (diethylstilbestrol, estrone, 17beta-estradiol, mestranol, 17alpha-ethinylestradiol and estriol) in water samples is described. Samples, up to 2000 ml, were concentrated using Oasis HLB solid-phase extraction cartridges. Analytes were derivatized with N-methyl-N-(trimethylsilyl)trifluoroacetamide and determined by GC-MS or GC-MS-MS. The reactivity of several silylation reagents versus aliphatic and aromatic hydroxyl groups contained in the structure of the selected analytes was evaluated. Influence of parameters such as sample pH, nature of the water samples and derivatization conditions on the performance of the whole analytical procedure was systematically studied. Under optimal conditions, quantification limits between 1 and 3 ng/l were achieved for the determination of the considered estrogens in sewage water.
This paper presents the development of an analytical procedure for the determination of two sexual steroid hormones: 17beta-estradiol and estrone, and the synthetic contraceptive estrogen, 17alpha-ethynylestradiol in effluents of wastewater treatment plants. Samples are extracted via solid-phase extraction using C18 cartridges. Extracts in ethyl acetate are then purified with a liquid-liquid separation with aqueous sodium chloride, then with a clean-up on a Florisil cartridge. Steroids are analyzed using an LC-MS-MS ion trap system. Internal quantification with the corresponding deuterated steroids leads to limits of quantification at 5 ng/l for estrone and 10 ng/l for estradiol and ethynylestradiol. In mineral spiked water, recoveries are 91% for 17beta-estradiol, 97% for estrone and 87% for 17alpha-ethynylestradiol and RSDs are 15% for 17beta-estradiol, 11% for estrone and 23% for 17alpha-ethynylestradiol.
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