Abstract
The presence of pesticide residues in water is a huge worldwide concern. In this paper we described the development and validation of a new liquid chromatography tandem mass spectrometric (LC-MS/MS) method for both screening and quantification of pesticides in water samples. In the sample preparation stage, the samples were buffered to pH 7.0 and pre-concentrated on polymeric-based cartridges via solid-phase extraction (SPE). Highly sensitive detection was carried out with mobile phases containing only 5 mM ammonium formate (pH of 6.8) as an eluent additive and using only positive ionization mode in MS/MS instrument. Hence, only 200-fold sample enrichment was required to set a screening detection limit (SDL) and reporting limit (RL) of 10 ng/L. The confirmatory method was validated at 10 and 100 ng/L spiking levels. The apparent recoveries obtained from the matrix-matched calibration (5–500 ng/L) were within the acceptable range (60–120%), also the precision (relative standard deviation, RSD) was not higher than 20%. During the development, 480 pesticides were tested and 330 compounds fulfilled the requirements of validation. The method was successfully applied to proficiency test samples to evaluate its accuracy. Moreover, the method robustness test was carried out using higher sample volume (500 mL) followed by automated SPE enrichment. Finally, the method was used to analyze 20 real samples, in which some compounds were detected around 10 ng/L, but never exceeded the assay maximum level.
Highlights
To protect crops from pathogens, fungi, weeds and insects, millions of tons of pesticides are applied each year in order to maintain agricultural productivity [1–4]
We report for the first time the simultaneous separation of more than 300 pesticides in ground- and surface water using a simple sample enrichment and LCMS/MS separation
The LC-MS/MS separation for 480 compounds in neat solvent (Figure S1 and Table S1) was developed for the analysis of large numbers of pesticides in food samples according to the EN 15662:2018 standard [26]
Summary
To protect crops from pathogens, fungi, weeds and insects, millions of tons of pesticides are applied each year in order to maintain agricultural productivity [1–4]. Hundreds of pesticides are registered in the European Union (EU) and most of them have maximum residue limits (MRLs) in foods of plant origin to protect consumers against toxic chemicals [6]. While many of these chemicals are readily degraded in the environment or have no adverse effects on human health, there are some for which there is little toxicological information [2–5,7–9]. There is a great need to monitor pesticide residues in water samples using state-of-the-art analytical techniques that enable the simultaneous analysis of high numbers of compounds [2]
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