engleski

Validation of multiresidue method for determination of multiclass pesticides in ground, surface and drinking water

Numerous pesticides have been widely used to prevent and treat plant diseases and pests in agricultural products and as a result, excessive residual pesticide content is frequently reported in ground, surface and drinking water sources. EEC Directive 98/83/EC has established a maximum allowed concentration of 100 ngL−1 for individual pesticides and related products, and of 500 ngL−1 for total pesticides in drinking water and 1000–3000 ngL−1 in surface water. To support the enforcement of this legislation, a reliable, simple and robust liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination 166 pesticides including carbamates, organophosphates, triazine and triazoles, imidazoles, etc. was validated and implemented in the routine monitoring and surveillance programme. Water samples were extracted using SPE method on HLB columns and eluted with methanol and ethyl-acetate. The trueness at three different concentrations of 25 ngL−1 , 100 ngL−1 and 150 ngL−1 over the analytical range varied between 89 and 122%. The limit of detection (LOD) and limit of quantification (LOQ) of the method were 10 ngL−1 and 25 ngL−1, respectively. Precision expressed as RDS (%) ranged from 1.9 to 24.9. The performance of the method was confirmed by the satisfactory results (z-scores < 2) of the proficiency testing organised by AGLAE (Round 17M65B) for all 34 pesticides and degradation residues found in tested river water sample. The method was accredited according to the HRN EN ISO 17025. The method has been used for the analysis of 532 both ground, surface and drinking water samples in the period from 2018.-2019.

Validation, pesticides, water, LC-MS/MS, SPE

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