Interlaboratory study on determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin in fish

An interlaboratory round robin study was carried out to estimate the reliability of data on 2,3,7,8-tetrachlorodibenzo-p-dioxin (TCDD) in fish. Using different methods, 13 laboratories (4 Canadian, 9 American) agreed to analyze 4 fish samples; 3 were Great Lakes salmonids containing bio-incurred levels of TCDD below 100 ppt and the fourth was an ocean fish fillet containing no measurable TCDD. Samples were sent as freeze-dried portions as it was shown that no change of TCDD occurred by this sample preparation. Results were normalized between laboratories by supplying each with an aliquot of the same 2,3,7,8-TCDD standard. Eight laboratories reported a set of results of which one set was rejected. Values from the 7 remaining laboratories for the 3 positive fish showed mean concentrations in pg/g (ppt) and (CV, %) of 61.2 (13.9), 30.4 (18.4), and 32.3 (25.4). Detection limits averaged 3.6 ppt and ranged between 1 and 10 ppt. No significant differences appeared in the concentration of 2,3,7,8-TCDD in fish samples from methods differing in the use of: (i) digestion or extraction techniques, (ii) high or low resolution mass spectrometry, and (iii) isomer specific or nonspecific separations. Overall recovery values using internal standards varied greatly (29-109%) even within the same laboratory and pointed to the need to use an internal standard to obtain precise results. Agreement among laboratories was good considering the level quantitated (ppt) and the diverse methodology.