Electron capture gas-liquid chromatographic determination of methyl mercury in fish and shellfish: collaborative...

A method for determining methyl mercury in fish and shellfish was collaboratively studied in 8 laboratories. Methyl mercury is isolated from acetone-washed, homogenized tissue by adding hydrochloric acid and extracting into benzene the methyl mercuric chloride that is formed. The benzene extract is concentrated and analyzed for methyl mercuric chloride by electron capture gas-liquid chromatography on 5% DEGS-PS treated with inorganic mercuric chloride solution. The quantitation limit for the method is 0.05 micrograms Hg/g. Each collaborator determined methyl mercury at 2 levels in blind duplicate samples of swordfish, tuna, oyster, and shrimp tissues. Both fortified and unfortified samples were analyzed. Methyl-bound mercury in the samples ranged from 0.15 to 2.48 micrograms Hg/g. The reproducibility coefficients of variation for the 8 samples ranged from 3 to 13%. The accuracy, measured by comparison to reference values, ranged from 99 to 120%. Reference values were determined in the Associate Referee's laboratory by replicate analyses of the fortified and unfortified samples. The method has been adopted official first action.