Estimating uncertainty in matrix solid phase extraction methodology for the determination of chlorinated compounds in fish

Abstract

In this study, a detailed process of uncertainty estimation associated with matrix solid phase dispersion method (MSPD) for the extraction of organochlorinated compounds from fish coupled with gas chromatography is given. The evaluation of uncertainty arising from trueness using fully nested experimental designs is presented by estimating proportional bias, in terms of recovery. The uncertainty of measurements associated with the actual chromatographic process was also estimated. The methodology was applied for the determination of selected organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in real fish samples, from selected study locations in Western Greece (Mesologgi lagoon and Trichonida lake), based on chromatographic techniques. The sources of uncertainty are presented along with the calculated combined uncertainty terms derived from the analytical procedure and chromatographic process. The estimation of uncertainty was included in the presentation of final determinations.

Keywords:

• matrix solid phase dispersion
• organochlorine pesticides
• polychlorinated biphenyls
• uncertainty

This work was first presented at the 7th European Conference on Pesticides and Related Organic Micropollutants in the Environment and 13th Symposium on Chemistry and Fate of Modern Pesticides, 7–10 October 2012, Porto, Portugal.