PMID- 16035353 OWN - NLM STAT- MEDLINE DCOM- 20051007 LR - 20190720 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1082 IP - 2 DP - 2005 Aug 5 TI - Microwave assisted extraction followed by gas chromatography with tandem mass spectrometry for the determination of triclosan and two related chlorophenols in sludge and sediments. PG - 128-35 AB - A procedure for the determination of 2-(2,4-dichlorophenoxy)-5-chlorophenol (Triclosan) and two possible transformation compounds, 2,4-dichlorophenol (2,4-DCP) and 2,4,6-trichlorophenol (2,4,6-TCP), in sludge from sewage treatment plants (STP) and sediments is presented. Extraction was performed using an acetone:methanol (1:1) mixture under the action of a microwave field. The centrifuged supernatant was diluted with a NaOH aqueous solution and twice extracted with n-hexane for removing neutral and basic interferences. The aqueous layer was acidified and processed as a waste water sample. After concentration analytes were silylated and determined by gas chromatography with tandem mass spectrometry (GC-MS/MS). Influence of experimental conditions on the yield of the extraction process and on the efficiency of the further clean-up step was thoroughly evaluated. Performance of MS/MS detection in comparison to single MS is described. Under final working conditions quantification limits between 0.4 and 0.8 ng/g and recoveries from 78% to 106% were obtained. The method was applied to the analysis of several sludge and sediment samples. Only low levels of TCS were detected in some of the sediments; however, all three compounds were found in sludge samples at concentrations ranging from 7 to 316 ng/g, in the case of chlorophenols, and from 420 to 5400 ng/g, for Triclosan. FAU - Morales, S AU - Morales S AD - Departamento de Quimica Analitica, Nutricion y Bromatologia, Instituto de Investigacin y Analisis Alimentario, Universidad de Santiago de Compostela, Santiago de Compostela 15782, Spain. FAU - Canosa, P AU - Canosa P FAU - Rodriguez, I AU - Rodriguez I FAU - Rubi, E AU - Rubi E FAU - Cela, R AU - Cela R LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Chlorophenols) RN - 0 (Sewage) RN - 4NM5039Y5X (Triclosan) RN - MHS8C5BAUZ (2,4,6-trichlorophenol) RN - R669TG1950 (2,4-dichlorophenol) SB - IM MH - Chemical Fractionation MH - Chlorophenols/*analysis MH - Gas Chromatography-Mass Spectrometry/*methods MH - Geologic Sediments/*chemistry MH - Microwaves MH - Reproducibility of Results MH - Sewage/*chemistry MH - Triclosan/*analysis EDAT- 2005/07/23 09:00 MHDA- 2005/10/08 09:00 CRDT- 2005/07/23 09:00 PHST- 2005/07/23 09:00 [pubmed] PHST- 2005/10/08 09:00 [medline] PHST- 2005/07/23 09:00 [entrez] AID - S0021-9673(05)01102-7 [pii] AID - 10.1016/j.chroma.2005.05.059 [doi] PST - ppublish SO - J Chromatogr A. 2005 Aug 5;1082(2):128-35. doi: 10.1016/j.chroma.2005.05.059.