Interlaboratory comparison study on PCDDs and PCDFs in cow's milk

Abstract

Six laboratories in four European countries (GER, GB, S, NL) have conducted an interlaboratory comparison study on the analysis of dioxins in cow's milk. The study comprised a cross comparison of standards and the analysis of the 2,3,7,8-substituted congeners of PCDD/Fs in three different milk pools (no spiking). Participants used their own procedures and methods for the determination of the fat content and PCDD/F levels in biological samples, all using non-polar gas chromatography and medium to high resolution mass spectrometry (RP=3.000–10.000). Quantification was performed by the use of a common quantification standard mixture of the native PCDD/Fs (4 labs) or the own quantification standards (2 labs). Within-laboratory reproducibilities for the determination of the major toxic congeners and the total TCDD toxicity equivalence (TE) level were between 2 and 16% (RSD) with a mean variation of 6% on TE basis. The interlaboratory comparison for TE values agreed within 10–17% (RSD) for TE values between 10.4 and 2.8 pg TE/g milk fat. Reliabilities of both participants and the common standards were difficult to assess and probably less good than expected. Differences in these standards were typically within 25% of expected concentrations up to 50% for some congeners by some laboratories.