PMID- 14658021 OWN - NLM STAT- MEDLINE DCOM- 20040715 LR - 20160512 IS - 1618-2642 (Print) IS - 1618-2642 (Linking) VI - 378 IP - 3 DP - 2004 Feb TI - Integrated procedure for determination of endocrine-disrupting activity in surface waters and sediments by use of the biological technique recombinant yeast assay and chemical analysis by LC-ESI-MS. PG - 697-708 AB - An integrated procedure using mass spectrometry and molecular biology for determination of estrogenicity in natural waters and sediments is reported. Solid-phase extraction (SPE) and pressurized-liquid extraction (PLE), respectively, were used for isolation of endocrine-disrupting compounds (EDC) from surface waters and sediments, followed by liquid chromatography-mass spectrometry using an electrospray interface (LC-ESI-MS). Twenty seven EDC were determined: non-ionic surfactants (nonylphenol ethoxylate), alkylphenols (e.g. nonylphenol and octylphenol), bisphenol A, phthalates, and natural and synthetic steroid sex hormones. Limits of detection varied from 0.02 to 0.22 microg L(-1) and from 1 to 10 microg kg(-1) in water and sediments, respectively. Recoveries ranged from 65 to 125% and 73 to 97% for waters and sediments, respectively. In addition to LC-ESI-MS determination, extracts obtained by SPE and PLE were analyzed by the recombinant yeast assay (RYA) to assess total estrogenic activity. This bioassay detects natural estrogens and xenoestrogens, producing a quantitative measurement of EDC irrespective of the identity of the chemical responsible for the activity. As a novelty, a relative estrogenicity factor was determined for 19 analytes with EC(50) values ranging from 10(-10) to 10(-9) mol L(-1) for synthetic estrogens, from 10(-7) to 10(-5) mol L(-1) for alkylphenol derivatives, and from 10(-5) to 10(-4) mol L(-1) for phthalates and benzothiazoles. By use of this integrated chemical-ecotoxicological approach good correlation was usually established between chemical composition and estrogenic effects for surface water and sediment samples from Portugal. Estrogenic activity observed was mainly attributed to the presence of nonylphenolic compounds (with concentrations of NP ranging from 0.1 up to 44 microg L(-1) in waters and up to 1172 microg kg(-1) in sediments), and to the sporadic presence of estrogens, detected at ng L(-1) levels. FAU - Cespedes, Raquel AU - Cespedes R AD - Department of Environmental Chemistry, IIQAB-CSIC, Jordi Girona 18-26, 08034 Barcelona, Spain. FAU - Petrovic, Mira AU - Petrovic M FAU - Raldua, Demetrio AU - Raldua D FAU - Saura, Ursula AU - Saura U FAU - Pina, Benjamin AU - Pina B FAU - Lacorte, Silvia AU - Lacorte S FAU - Viana, Paula AU - Viana P FAU - Barcelo, Damia AU - Barcelo D LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20031205 PL - Germany TA - Anal Bioanal Chem JT - Analytical and bioanalytical chemistry JID - 101134327 RN - 0 (Water Pollutants, Chemical) SB - IM MH - Chromatography, High Pressure Liquid/*methods MH - Endocrine Glands/*drug effects MH - Geologic Sediments/chemistry MH - Recombination, Genetic MH - Reference Standards MH - Saccharomyces cerevisiae/*genetics MH - Sensitivity and Specificity MH - Spectrometry, Mass, Electrospray Ionization/*methods MH - Water Pollutants, Chemical/*analysis/toxicity EDAT- 2003/12/06 05:00 MHDA- 2004/07/16 05:00 CRDT- 2003/12/06 05:00 PHST- 2003/05/23 00:00 [received] PHST- 2003/09/12 00:00 [revised] PHST- 2003/09/22 00:00 [accepted] PHST- 2003/12/06 05:00 [pubmed] PHST- 2004/07/16 05:00 [medline] PHST- 2003/12/06 05:00 [entrez] AID - 10.1007/s00216-003-2303-5 [doi] PST - ppublish SO - Anal Bioanal Chem. 2004 Feb;378(3):697-708. doi: 10.1007/s00216-003-2303-5. Epub 2003 Dec 5.