Intercomparison study for the determination of selected polychlorinated biphenyls (PCBs) in feed matrices

Abstract.

Analytical methodology currently employed for the determination of seven indicator PCBs in three compound feeds and fish meal has been evaluated in a collaborative study. The majority of the obtained relative standard deviations of the PCBs varied from 20 to 30%. On assuming a target relative standard deviation of 22% for the analytical results, statistical evaluation showed that about 80% of the participating laboratories delivered data within an acceptable range of ±44% of the assigned concentration in the test materials. However, between 10 and 20% of the participating laboratories reported unacceptable results. Major problems seemed to arise from insufficient separation of PCB congeners, low extraction efficiency, and calculation errors. Correct identification of the target PCB congeners was a prevalent problem if only one capillary column in combination with an electron capture detector (ECD) was employed. The correct preparation of the calibration solution by the laboratories turned out to be only a minor problem. The laboratories participating in this study employed quite different techniques at all stages of the analytical procedure. Principal component analysis indicated that laboratories using an internal standard tended to report higher values for the target analytes. If the PCB concentrations were related to the fat content of the sample, the variability of the reported results decreased for compound feed but increased for fish meal. These inconsistent results are probably due to the fact that fat is not an objective parameter but is defined by the analytical technique employed. It is assumed that harmonizing analytical methods for the determination of this parameter could improve the precision of the PCB results.