TY - JOUR AU - Jókainé Szatura, Zsuzsa AU - Abrankó, László AU - Fodor, Péter TI - SPME-GC-pyrolysis-AFS determination of methylmercury in marine fish products by alkaline sample preparation and aqueous phase phenylation derivatization JF - JOURNAL OF AGRICULTURAL AND FOOD CHEMISTRY J2 - J AGR FOOD CHEM VL - 53 PY - 2005 IS - 14 SP - 5499 EP - 5505 PG - 7 SN - 0021-8561 DO - 10.1021/jf0501140 UR - https://m2.mtmt.hu/api/publication/1390070 ID - 1390070 AB - Characterization of a cost-efficient analytical method based on alkaline sample digestion with KOH and NaOH, followed by aqueous phase phenylation derivatization with NaBPh4 and solid phase microextraction (SPME) for the determination of methylmercury in typical fish-containing food samples commercially available in Hungary, is reported. The sample preparation procedure along with the applied SPME-GC-pyrolysis-AFS system was validated by measuring certified reference materials (CRM) BCR-464, TORT-2, and a candidate CRM BCR 710. To carry out an estimation of average Hungarian methylmercury exposures via marine fish and/or fish-containing food consumption, 16 commercially available products and 3 pooled representative seafood samples of-according to a previous European survey-the three most consumed fish species in Hungary, herring, sardines, and hake, were analyzed. Methylmercury concentrations of the analyzed samples were in the range 0.016-0.137 mu g of MeHg g(-1) dry weight as Hg. LA - English DB - MTMT ER - TY - JOUR AU - Grinberg, P. AU - Campos, R.C. AU - Mester, Zoltán AU - Sturgeon, R.E. TI - A comparison of alkyl derivatization methods for speciation of mercury based on solid phase microextraction gas chromatography with furnace atomization plasma emission spectrometry detection JF - JOURNAL OF ANALYTICAL ATOMIC SPECTROMETRY J2 - J ANAL ATOM SPECTROM VL - 18 PY - 2003 IS - 8 SP - 902 EP - 909 PG - 8 SN - 0267-9477 DO - 10.1039/b212545e UR - https://m2.mtmt.hu/api/publication/30393739 ID - 30393739 N1 - Institute for National Measurements Standards, National Research Council of Canada, Ottawa, Ont. K1A 0R6, Canada Department of Chemistry, Pontificia Universidade Católica do Rio de Janeiro, Rua Marques de Sao Vicente, 225, 22453-900 Rio de Janeiro-RJ, Brazil Cited By :50 Export Date: 15 January 2019 Correspondence Address: Sturgeon, R.E.; Institute for National Measurements Standards, National Research Council of Canada, Ottawa, Ont. K1A 0R6, Canada; email: ralph.sturgeon@nrc.ca AB - Several derivatizing agents were evaluated for use in speciating mercury in biological samples using solid phase microextraction in conjunction with tandem gas chromatography-furnace atomization plasma emission spectrometry (SPME-GC-FAPES). Following digestion with methanolic potassium hydroxide, the pH of the samples was adjusted and NaCl added when necessary. The mercury species were then derivatized with sodium tetraphenylborate or sodium tetrapropylbqrate and extracted by SPME using a 100 um PDMS coated fiber. The derivatized species were then separated by GC and detected by FAPES. All experimental parameters were optimized for best separation and analytical response. Propylation proved to be more sensitive, robust and faster than ethylation or phenylation, leading to procedural detection limits of 0.55 ng g-1 for methylmercury, 0.34 ng g-1 for ethylmercury and 0.23 ng g-1 for inorganic mercury. An intra-day and intra-fiber precision of typically 2.2% was achieved whereas long-term (4 months) and inter-fiber reproducibility precision was typically 4.4%. The accuracy of the method was validated by the analysis of Certified Reference Materials (DORM-2, DOLT-2 and TORT-2) from the National Research Council of Canada. © The Royal Society of Chemistry 2003. LA - English DB - MTMT ER - TY - JOUR AU - Grinberg, P. AU - Campos, R.C. AU - Mester, Zoltán AU - Sturgeon, R.E. TI - Solid phase microextraction capillary gas chromatography combined with furnace atomization plasma emission spectrometry for speciation of mercury in fish tissues JF - SPECTROCHIMICA ACTA PART B-ATOMIC SPECTROSCOPY J2 - SPECTROCHIM ACTA B VL - 58 PY - 2003 IS - 3 SP - 427 EP - 441 PG - 15 SN - 0584-8547 DO - 10.1016/S0584-8547(02)00272-0 UR - https://m2.mtmt.hu/api/publication/30393749 ID - 30393749 AB - The use of solid phase microextraction in conjunction with tandem gas chromatography-furnace atomization plasma emission spectrometry (SPME-GC-FAPES) was evaluated for the determination of methylmercury and inorganic mercury in fish tissue. Samples were digested with methanolic potassium hydroxide, derivatized with sodium tetraethylborate and extracted by SPME. After the SPME extraction, species were separated by GC and detected by FAPES. All experimental parameters were optimized for best separation and analytical response. A repeatability precision of typically 2% can be achieved with long-term (3 months) reproducibility precision of 4.3%. Certified Reference Materials DORM-2, DOLT-2 and TORT-2 from the National Research Council of Canada were analyzed to verify the accuracy of this technique. Detection limits of 1.5 ng g-1 for methylmercury and 0.7 ng g-1 for inorganic mercury in biological tissues were obtained. © 2002 Elsevier Science B.V. All rights reserved. LA - English DB - MTMT ER -