作者: Daniel S. Vidler , Richard O. Jenkins , John F. Hall , Chris F. Harrington
DOI: 10.1002/AOC.1173
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摘要: The use of high-performance liquid chromatography (HPLC) coupled to inductively plasma mass spectrometry (ICP-MS) for the determination methylmercury (MeHg+) in fish tissue and hair samples is described. Analysis these sample types required when carrying out biomonitoring studies determine human dietary exposure this toxic mercurial compound. developed method used a mobile phase containing an organic modifier sulfydryl compound (1:1 v/v methanol:water 0.01% 2-mercaptoethanol) limit peak tailing aid separation. chromatographic separation was ICP-MS detector via short piece PEEK tubing, attached nebulizer. A cooled spraychamber oxygen addition post-nebulization were solvent loading on reduce carbon build-up cones, respectively. preparation procedure employed drying step followed by digestion using tetramethylammonium hydroxide (TMAH) heating open vessel microwave system. Two certified reference materials (CRM), tuna CRM 463 464 (BCR, Brussels), proficiency test sample, IMEP-20 (IRMM, Geel, Belgium) NIES no. 13 (National Institute Environmental Science, Japan), evaluate method. recovery MeHg+ four between 83 100%, with precisions better than 6% three separate extractions different materials. quantitation protocol 0.5 µg Hg g−1. stability extracts also assessed losses 14–16% observed after storage refrigerator at 5 °C, high-density polypropylene tubes, 6 months. has been previously atmospheric pressure ionization (API-MS) provide structural characterization calibration isotope dilution (IDMS) high accuracy quantitation. Copyright © 2006 John Wiley & Sons, Ltd.