PMID- 16233867 OWN - NLM STAT- MEDLINE DCOM- 20060214 LR - 20131121 IS - 0021-9673 (Print) IS - 0021-9673 (Linking) VI - 1093 IP - 1-2 DP - 2005 Nov 4 TI - Determination of mercury species in fish reference materials by gas chromatography-atomic fluorescence detection after closed-vessel microwave-assisted extraction. PG - 21-8 AB - A simple and rapid method has been developed for speciation analysis of inorganic mercury and monomethylmercury (MMHg) in biological tissues. The procedure is based on the quantitative closed-vessel microwave-assisted leaching of mercury from biological samples with an alkaline extractant. The extracted mercury species are ethylated and analysed by capillary gas chromatography coupled to an atomic fluorescence detector via pyrolysis (CGC-pyro-AFS). The coupling between capillary gas chromatography and atomic fluorescence detector was optimized with the aim of minimizing the detection limits and time necessary for the species-selective determination of mercury compounds. The use of closed-vessel microwave-assisted extraction along with no clean-up steps before the ethylation leads to a significant total analysis time decrease with respect to similar procedures. The detection limit was 2 pg for MMHg (as Hg) and 1 pg for inorganic mercury. The method was validated by the analysis of DORM-2 (dogfish muscle) and DOLT-3 (dogfish liver) certified reference materials. The inorganic mercury and methylmercury concentrations found were in good agreement with the certified values. Recovery studies of fish muscle tissue spiked with inorganic mercury and MMHg were done to check the reliability of the method. In all cases satisfactory recoveries (92-105%) were obtained. FAU - Nevado, Juan Jose Berzas AU - Nevado JJ AD - Regional Institute for Applied Scientific Research, University of Castilla-La Mancha, E-16071 Ciudad Real, Spain. FAU - Martin-Doimeadios, Rosa Carmen Rodriguez AU - Martin-Doimeadios RC FAU - Bernardo, Francisco Javier Guzman AU - Bernardo FJ FAU - Moreno, Maria Jimenez AU - Moreno MJ LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20050826 PL - Netherlands TA - J Chromatogr A JT - Journal of chromatography. A JID - 9318488 RN - FXS1BY2PGL (Mercury) SB - IM MH - Animals MH - Chromatography, Gas/*methods MH - *Dogfish MH - Mercury/*analysis/classification MH - Microwaves MH - Reference Standards MH - Reproducibility of Results MH - Sensitivity and Specificity MH - Spectrometry, Fluorescence/*methods EDAT- 2005/10/20 09:00 MHDA- 2006/02/16 09:00 CRDT- 2005/10/20 09:00 PHST- 2005/05/23 00:00 [received] PHST- 2005/07/12 00:00 [revised] PHST- 2005/07/18 00:00 [accepted] PHST- 2005/10/20 09:00 [pubmed] PHST- 2006/02/16 09:00 [medline] PHST- 2005/10/20 09:00 [entrez] AID - S0021-9673(05)01554-2 [pii] AID - 10.1016/j.chroma.2005.07.054 [doi] PST - ppublish SO - J Chromatogr A. 2005 Nov 4;1093(1-2):21-8. doi: 10.1016/j.chroma.2005.07.054. Epub 2005 Aug 26.