Comprehensive multiresidue chromatographic methods for monitoring pesticides in agricultural areas and corresponding plant protection zones.

This article reports a comprehensive analytical method for the identification and quantification of a broad range of pesticides in green plant crops. The sample preparation method for pesticides involved an optimization of the QuEChERS-based extraction protocol, with sample mass, volume of added water, and the type of cleanup sorbent as variables. A sorbent combination based on ENVI-Carb and ChloroFiltr was examined. A highly efficient method was developed for the purification of plant extracts with 900 mg MgSO4, 150 mg PSA, and 15 mg ENVI-Carb at the d-SPE stage, combined with gas chromatography and liquid tandem mass spectrometry for the determination of 197 pesticides in crop plants containing chlorophyll. The method was validated in accordance with the requirements of international guidelines SANTE/11312/2021. The method was applied to quantify pesticide residues in 29 pairs of green crop plants and plants from the corresponding crop protection zone to verify whether the zones are effective barriers to prevent pesticides from penetrating outside agricultural areas. The number and types of agrochemical preparations were chosen by farmers. In total, more than 60 one- and several-component pesticide formulations were applied to the crops included in the study. The pesticide residues were detected in 21 crop samples and 3 samples from protection zones. Epoxiconazole, an active substance that was banned for use in 2021, was found in a spring barley sample. Based on the conducted research, the effectiveness of the protection zones has been clearly demonstrated, and it has been proven that environmental migration of pesticides and unauthorized agricultural practices pose a risk to ecosystems.

Rapid MSPD-LC-MS/MS Procedure for Determination of Pesticides in Potato Tubers.

The program of potato protection recommended by the producers of agrochemicals requires application: thiamethoxam, lambda-cyhalothrin, deltamethrin, rimsulfuron and metalaxyl. Therefore, there is a risk that these pesticides are present in tubers, thus posing a toxicological risk to the consumer. In this respect, it is necessary to monitor the presence of these compounds in edible plants. Therefore, the aim of this paper was to develop a novel, simple and robust analytical procedure for simultaneous determination of above-mentioned pesticides in potato tubers. To develop an analytical procedure that fulfills SANTE demands, quick, easy, cheap, effective, rugged and safe method and matrix solid phase dispersion technique were investigated. The final determination was conducted by liquid chromatography with tandem mass spectrometry. The obtained experimental data were analyzed by analysis of variance. For the extraction of analytes, matrix solid phase dispersion with octadecyl sorbent and methanol as eluent was chosen, since it provides the validation parameters according to SANTE requirements (recovery: 77-111%, relative standard deviation: 1-10%, limit of quantification: 0.9-5.0 µg/kg). This innovative analytical procedure is a practical analytical tool, which was successfully proven by applying it for target pesticides determination in potato tuber samples of different varieties randomly chosen at local markets.