Analysis of Multiresidue Pesticides in Agricultural Paddy Soils Near Industrial Areas in Korea by GC–MS/MS and LC–MS/MS Using QuEChERS Extraction with dSPE Clean-Up

Pesticides have been used to control pests in agricultural fields and storage systems before circulating agricultural products to markets. A tandem mass spectrometry, equipped with gas chromatographic separation (GC–MS/MS) or ultra-performance liquid chromatographic separation (LC–MS/MS), was used to monitor residual pesticides in Korean rice paddy soils. Selective multiple reaction monitoring was employed during the analyses to achieve multiresidue pesticide analysis using GC–MS/MS and LC–MS/MS of 342 pesticides. In this study, QuEChERS extraction was employed with a dSPE clean-up to establish an effective pretreatment process. The limit of detection (LOD) and limit of quantification (LOQ) were set up for all pesticides, and method validation was performed for linearity and recovery at levels of 10 and 50 mg kg−1 in the untreated soil sample. All pesticides satisfied the acceptable recovery range of 70–120%, within less than 20% RSD values, except for ametoctradin and gibberellic acid. In the paddy soil analyses, tricyclazole was the most frequently detectable pesticide, followed by oxadiazon, endosulfan, and chlorantraniliprole. Continuous monitoring of residual pesticides in paddy soils should be conducted due to the translocation of some systemic pesticides from soils to crop plants, and the impact of residual pesticides on the environment.

Pesticide Residue Analysis in Fruit- and Vegetable-Based Baby Foods Using GC-Orbitrap MS

This paper presents an efficiency evaluation of GC coupled with quadrupole Orbitrap MS for identification and quantitation in the multiresidue pesticide analysis of baby foods in full-scan mode. The identification criteria were studied following SANTE guidelines (retention time, mass accuracy, and ion ratio), comfortably complying with the values established, even at 0.003 mg/kg. Method validation was carried out on 15 selected GC-amenable pesticides covered by Commission Directive No. 2006/125/EC in three different baby food matrixes. Recovery studies were performed at 0.003 and 0.006 mg/kg, with 96% of the cases falling within the 70–120% range and with RSDs <15% for all the pesticides assayed. Linearity over 3 orders of magnitude was verified, with residuals <16% and correlation coefficient values >0.995. In general, matrix effect values were >100%. The LOQ was 0.003 mg/kg for 97% of the cases. The validated method was applied to 20 real baby food samples from Spain and to the European Union Proficiency Test FV-BF01 sample, in which the z-scores obtained were <1, thus demonstrating that this instrumentation has good quantitation capabilities.