Occurrence of pesticides in Dutch drinking water sources

We determined pesticide occurrence in groundwater and surface water sources used for drinking water production in The Netherlands, using both routine monitoring data from Dutch drinking water companies and by studying the presence of newly authorized pesticides in drinking water sources. An analytical LC-MS/MS method was developed for 24 recently authorized pesticides, selected based on their mobility and persistence, and applied in a Dutch/Belgian ground- and surface water monitoring campaign. 15 of these pesticides were detected, including seven in concentrations above the water quality standard from the Water Framework Directive. Two neonicotinoids were detected in highest concentrations: acetamiprid (1.1 μg/L) and thiamethoxam (0.4 μg/L). The routine monitoring data was collected over 2010–2014 in The Netherlands, covering 408 pesticides and 52 metabolites. 63 pesticides and 6 metabolites were prioritized according to their presence in groundwater, surface water and drinking water. The vast majority of the pesticides in routine monitoring has not been detected or only in low concentrations. Overall, the study shows that pesticides are of major concern in drinking water sources across the Netherlands. In two third of the abstraction areas pesticides and/or metabolites have been detected. In one third of the abstraction areas pesticide and/or metabolites concentration exceeded water quality standards according to the Water Framework Directive. The results emphasize that monitoring should focus on priority pesticides, since the vast majority of the pesticides has a low priority. The occurrence of recently authorized pesticides in drinking water sources demonstrates the importance to keep routine monitoring methods up to date

Determination of nifursol metabolites in poultry muscle and liver tissue: development and validation of a confirmatory method

A method is described for the identification and quantitative determination of 3,5-dinitrosalicylic acid hydrazide (DSH), the marker residue of nifursol metabolites in poultry (turkey, broiler) muscle and liver tissue. The method is based on the acid-catalysed hydrolysis of tissue-bound metabolites to free DSH and in situ derivatisation with 2-nitrobenzaldehyde to the corresponding nitrophenyl derivative NPDSH. A structural analogue of DSH, 4-hydroxy-3,5-dinitrobenzoic acid hydrazide (HBH) was synthesised to serve as an internal standard. The analytes were isolated from the matrix by liquid¿liquid extraction with ethyl acetate. Determination was performed by LC-MS/MS with negative electrospray ionisation. The [M ¿ H]+ ions of NPDSH and NPHBH at m/z 374 were fragmented by collision induced dissociation (CID) producing transition ions at m/z 182, 183 and 226. The transition ions at m/z 182 and 226 were selected for monitoring of NPDSH while the transition ion at m/z 183 was selected for NPHBH. The method has been validated according to the EU criteria of Commission Decision 2002/657/EC at 0.5, 1.0 and 1.5 µg kg¿1 in muscle and liver tissue. A decision limit (CC) was obtained of 0.04 and 0.025 µg kg¿1 in muscle and liver, respectively. Similarly a detection capability (CC) was obtained of 0.10 and 0.05 µg kg¿1 in muscle and liver, respectively. The introduction of HBH as an internal standard did not lead to a significant improvement of the quantitative performance of the method. In fact for liver better performance characteristics were obtained when the IS was not taken into account. Nevertheless, as a qualitative marker for recovery, HBH could still be very useful in the analysis of unknown sample