PMID- 18031005 OWN - NLM STAT- MEDLINE DCOM- 20080205 LR - 20131121 IS - 0021-8561 (Print) IS - 0021-8561 (Linking) VI - 55 IP - 25 DP - 2007 Dec 12 TI - Online YPA4 resin microcolumn separation/preconcentration coupled with inductively coupled plasma optical emission spectrometry (ICP-OES) for the speciation analysis of mercury in seafood. PG - 10129-34 AB - A simple and effective method for the determination of trace amounts of methylmercury (MeHg(+)) and inorganic mercury (Hg(2+)) in seafood was developed by online microcolumn separation/preconcentration combined with inductively coupled plasma optical emission spectrometry (ICP-OES). It was found that Hg(2+) could be quantitatively adsorbed by YPA 4 resin from pH 7.0 to strong acidic medium (6 mol L(-1) HCl) and that MeHg(+) was retained by the YPA 4 microcolumn only at pH 1.0-7.0. Therefore, a strong acidic medium (about 5 mol L(-1) HCl), which could liberate mercury species from biological samples, was used to directly separate inorganic Hg(2+) from total Hg, and MeHg(+) in effluent was retained by YPA 4 column after the effluent was adjusted to pH 1.5. The effects of acidity, sample flow rate and volume, elution solution, and interfering ions on recovery of the two mercury species have been systematically investigated. Under optimal conditions, the limits of detection (LODs) were 72 and 44 ng L(-1) for Hg(2+) and MeHg(+) (as Hg) with online concentration factors of 12.5 and 12.1, respectively. The relative standard deviations (RSDs) for nine replicate determinations at 5 ng mL(-1) levels of mercury species were 2.7 and 2.0% for Hg(2+) and MeHg(+), respectively. The calibration graphs were linear with a correlation coefficient of 0.9902 in the range of 0.5-100 ng mL(-1) for Hg(2+) and 0.9976 in the range of 0.1-100 ng mL(-1) for MeHg(+), respectively. The developed method was successfully applied to the direct determination of MeHg(+) and Hg(2+) in seafood samples, and the recoveries for the spiked samples were in the range of 89.9-102.4% (MeHg(+)) and 87.0-104.6% (Hg(2+)), respectively. The method was validated by analyzing a certified reference material DORM-2 (dogfish muscle), and the determined values were in good agreement with certified values. FAU - Xiong, Chaomei AU - Xiong C AD - Department of Chemistry, Wuhan University, Wuhan 430072, People's Republic of China. FAU - Hu, Bin AU - Hu B LA - eng PT - Journal Article PT - Research Support, Non-U.S. Gov't DEP - 20071122 PL - United States TA - J Agric Food Chem JT - Journal of agricultural and food chemistry JID - 0374755 RN - 0 (Cations, Divalent) RN - 0 (Chelating Agents) RN - 0 (Methylmercury Compounds) RN - FXS1BY2PGL (Mercury) RN - GYV9AM2QAG (Thiourea) SB - IM MH - Cations, Divalent/analysis MH - Chelating Agents MH - Chromatography/methods MH - Hydrogen-Ion Concentration MH - Mercury/*analysis MH - Methylmercury Compounds/analysis MH - Seafood/*analysis MH - Spectrum Analysis/methods MH - Thiourea EDAT- 2007/11/23 09:00 MHDA- 2008/02/06 09:00 CRDT- 2007/11/23 09:00 PHST- 2007/11/23 09:00 [pubmed] PHST- 2008/02/06 09:00 [medline] PHST- 2007/11/23 09:00 [entrez] AID - 10.1021/jf071979b [doi] PST - ppublish SO - J Agric Food Chem. 2007 Dec 12;55(25):10129-34. doi: 10.1021/jf071979b. Epub 2007 Nov 22.