摘要

A method for organic, inorganic and total mercury determination in fish tissue has been developed using chemical vapor generation and collection of mercury vapor on a gold gauze inside a graphite tube and further atomization by electrothermal atomic absorption spectrometry. After drying and cryogenic grinding, potassium bromide and hydrochloric acid solution (I mol L(-1) KBr in 6 mol L(-1) HCl) was added to the samples. After centrifugation, total mercury was determined in the supernatant. Organomercury compounds were selectively extracted from KBr solution using chloroform and the resultant solution was back extracted with 1% m/v L-cysteine. This solution was used for organic Hg determination. Inorganic Hg remaining in KBr solution was directly determined by chemical vapor generation electrothermal atomic absorption spectrometry. Mercury vapor generation from extracts was performed using I mol L(-1) HCl and 2.5% m/v NaBH(4) solutions and a batch chemical vapor generation system. Mercury vapor was collected on the gold gauze heated resistively at 80 degrees C and the atomization temperature was set at 650 degrees C. The selectivity of extraction was evaluated using liquid chromatography coupled to chemical vapor generation and determination by inductively coupled plasma mass spectrometry. The proposed method was applied for mercury analysis in shark, croaker and tuna fish tissues. Certified reference materials were used to check accuracy and the agreement was better than 95%. The characteristic mass was 60 pg and method limits of detection were 5, 1 and 1 ng g(-1) for organic, inorganic and total mercury, respectively. With the proposed method it was possible to analyze up to 2, 2 and 6 samples per hour for organic. inorganic and total Hg determination, respectively.

  • 出版日期2009-6