PMID- 2708292 OWN - NLM STAT- MEDLINE DCOM- 19890526 LR - 20161123 IS - 0004-5756 (Print) IS - 0004-5756 (Linking) VI - 72 IP - 2 DP - 1989 Mar-Apr TI - Determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin in fish, using electron capture gas chromatography with confirmation by mass spectrometry: interlaboratory study. PG - 394-8 AB - An interlaboratory study of the determination of 2,3,7,8-tetrachlorodibenzo-p-dioxin (2,3,7,8-TCDD) in fish was conducted by 6 analysts in 4 laboratories using high resolution gas chromatography with electron capture detection (HRGC-EC) for quantitative screening analysis. Samples consisted of 3 Great Lakes channel catfish homogenates containing different levels of bioincurred 2,3,7,8-TCDD; 1 of these was prepared in duplicate and another was prepared both with and without standard 2,3,7,8-TCDD fortification for a total of 5 samples per set. All methods used included addition of 1,3,7,8-TCDD surrogate (to correct for procedural losses) followed by ethanolic KOH digestion and hexane extraction. Certain cleanup steps used, including sulfuric acid washing and multidimensional column liquid chromatographic procedures, varied among laboratories. Mean HRGC-EC results for the bioincurred residues were 56.6, 25.2, and 7.7 pg/g (ppt) with corresponding relative standard deviations (RSDs) of 9.1, 18.6, and 53.2%. Average determination of standard 2,3,7,8-TCDD from the fortified sample (corrected for surrogate recoveries averaging 74.6%) was 106% of the added amount (30.9 pg/g) with 11.0% RSD. HRGC-multiple ion detection mass spectrometry (MS), monitoring 12 ions, was used for confirmation. With the exception of several results from 1 analyst, HRGC-MS and HRGC-EC quantitations were in good agreement. All but 1 result reported met all of the MS identity criteria. FAU - Fehringer, N V AU - Fehringer NV AD - Food and Drug Administration, Pesticides and Industrial Chemicals Research Center, Detroit, MI 48207. FAU - Walters, S M AU - Walters SM FAU - Niemann, R A AU - Niemann RA LA - eng PT - Journal Article PL - United States TA - J Assoc Off Anal Chem JT - Journal - Association of Official Analytical Chemists JID - 7505559 RN - 0 (Dioxins) RN - 0 (Polychlorinated Dibenzodioxins) SB - IM MH - Animals MH - Chromatography, Gas MH - Dioxins/*analysis MH - *Fishes MH - Mass Spectrometry MH - Polychlorinated Dibenzodioxins/*analysis EDAT- 1989/03/01 00:00 MHDA- 1989/03/01 00:01 CRDT- 1989/03/01 00:00 PHST- 1989/03/01 00:00 [pubmed] PHST- 1989/03/01 00:01 [medline] PHST- 1989/03/01 00:00 [entrez] PST - ppublish SO - J Assoc Off Anal Chem. 1989 Mar-Apr;72(2):394-8.