In-house validation of a simplified method for the determination of PCBs in food and feedingstuffs

This paper comprises a simplified method for the determination of polychlorinated biphenyls (PCBs) in food and feedingstuffs. The method includes a cold column extraction step, a simple clean-up with concentrated sulfuric acid, and a final determination of the PCBs using gas chromatography-mass spectrometry (GC/MS). An in-house validation study was performed to establish method performance characteristics such as decision limit, detection capability, trueness and precision of the method. To determine these characteristics both certified reference materials and spiked samples were utilized. The decision limit and the detection capability of the individual PCB congeners in food were 2 ng/g and 3 ng/g fat, respectively, while corresponding figures for feedingstuffs were 7 ng/g and 9 ng/g fat, respectively. The coefficient of variation (CV) varied from 2% to 5% for food on the 10 ng/g fat level and from 2% to 6% for feedingstuffs on the 25 ng/g fat level. The recoveries of the individual PCB congeners varied from 88% to 107%, indicating good correspondence with internationally recognized criteria for the performance characteristics of analytical methods. The robustness of the method was investigated by employing a factorial design methodology to determine the influence of six experimental factors on the results of the analysis. This clearly demonstrated that the method is fit for surveillance of PCBs in food and feedingstuffs, even though some care has to be taken with the solvent volume during the cold column extraction step as well as the addition of the standard to the sample. Additionally, the investigation clearly demonstrates that in-house validation approaches may be used for determination of the overall performance of analytical methods.