PMID- 17386931 OWN - NLM STAT- MEDLINE DCOM- 20070621 LR - 20090115 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1149 IP - 2 DP - 2007 May 18 TI - Optimisation of a microwave-assisted extraction method for the simultaneous determination of haloanisoles and halophenols in cork stoppers. PG - 138-44 AB - This study presents a method based on the use of microwave-assisted extraction (MAE) for the quantitative analysis of 2,4,6-trichloroanisole (TCA), 2,3,4,6-tetrachloroanisole (TeCA), pentachloroanisole (PCA), 2,4,6-tribromoanisole (TBA), 2,4,6-trichlorophenol (TCP), 2,3,4,6-tetrachlorophenol (TeCP), pentachlorophenol (PCP) and 2,4,6-tribromophenol (TBP) in cork stoppers. The influential parameters of the MAE procedure (extraction time, temperature and solvent volume) were optimised using a central composite experimental design combined with desirability functions. The optimal conditions identified were temperature 170 degrees C, solvent volume 35 mL and extraction time 90 min. MAE extracts were concentrated and derivatised prior to separation and quantification by gas chromatography with electron capture detection. To evaluate the applicability of the proposed MAE method, recovery results were compared with those obtained with the Soxhlet extraction method; the results were similar with both extraction methods. The new method was also satisfactorily applied to real cork stopper samples. FAU - Pizarro, C AU - Pizarro C AD - Department of Chemistry, University of La Rioja, C/Madre de Dios 51, 26006 Logrono, La Rioja, Spain. consuelo.pizarro@dq.unirioja.es FAU - Perez-del-Notario, N AU - Perez-del-Notario N FAU - Gonzalez-Saiz, J M AU - Gonzalez-Saiz JM LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20070319 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - 0 (Anisoles) RN - 0 (Halogens) RN - 0 (Phenols) SB - IM MH - Anisoles/*analysis MH - Halogens/*analysis MH - *Microwaves MH - Phellodendron/*chemistry MH - Phenols/*analysis MH - Reference Standards EDAT- 2007/03/28 09:00 MHDA- 2007/06/22 09:00 CRDT- 2007/03/28 09:00 PHST- 2007/01/25 00:00 [received] PHST- 2007/03/07 00:00 [revised] PHST- 2007/03/09 00:00 [accepted] PHST- 2007/03/28 09:00 [pubmed] PHST- 2007/06/22 09:00 [medline] PHST- 2007/03/28 09:00 [entrez] AID - S0021-9673(07)00495-5 [pii] AID - 10.1016/j.chroma.2007.03.055 [doi] PST - ppublish SO - J Chromatogr A. 2007 May 18;1149(2):138-44. doi: 10.1016/j.chroma.2007.03.055. Epub 2007 Mar 19.