Solid phase microextraction capillary gas chromatography combined with furnace atomization plasma emission spectrometry for speciation of mercury in fish tissues

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.