Dataset Information

Supporting dataset on the optimization and validation of a QuEChERS-based method for the determination of 218 pesticide residues in clay loam soil.

ABSTRACT: The dataset presented in this article supports "Optimization and validation of a method for the simultaneous environmental monitoring of 218 pesticide residues in clay loam soil" [1]. A method based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged & Safe) for the extraction of pesticide and some metabolites residues was developed. The quantification of the chemicals was performed by a combination of two complementary LC-MS/MS and GC-MS/MS analyses. Detailed optimization data of the QuEChERS extraction method is provided, including (1) salt combination, (2) acidification of the solvent (3) the amount of the selected acid (Formic Acid, FA) and (4) moisturization of the soil samples prior to extraction. In addition, all the validation data are presented, including the matrix effect, which was evaluated for each analyte using the recommended procedure.

SUBMITTER: Acosta-Dacal A

PROVIDER: S-EPMC7596106 | biostudies-literature | 2020 Dec

REPOSITORIES: biostudies-literature

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Supporting dataset on the optimization and validation of a QuEChERS-based method for the determination of 218 pesticide residues in clay loam soil.

Acosta-Dacal Andrea A Rial-Berriel Cristian C Díaz-Díaz Ricardo R Bernal Suárez Mª Del Mar MDM Zumbado Manuel M Henríquez-Hernández Luis Alberto LA Luzardo Octavio P OP

Data in brief 20201009

The dataset presented in this article supports "Optimization and validation of a method for the simultaneous environmental monitoring of 218 pesticide residues in clay loam soil" [1]. A method based on QuEChERS (Quick, Easy, Cheap, Effective, Rugged & Safe) for the extraction of pesticide and some metabolites residues was developed. The quantification of the chemicals was performed by a combination of two complementary LC-MS/MS and GC-MS/MS analyses. Detailed optimization data of the QuEChERS ex ...[more]

PMID: 33145377

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Project description:Commercial viticulture necessitates regular pesticide applications to manage diseases and pests, raising significant concerns regarding pesticide residues among stakeholders. Due to health risks associated with these residues in Turkish vine leaves, the European Commission has increased the frequency of official control from 20% to 50%. Thus, the aim of this study was to determine multi-class pesticide residues in brined vine leaves from Turkey. A total of 766 samples of vine leaves were collected between May 2022 and June 2023. More than 500 residues were analyzed using the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method, followed by liquid chromatography-tandem mass spectrometry. In-house validation data demonstrated that the analytical method exhibits fit-for-purpose performance in terms of linearity, accuracy, precision, and measurement uncertainty. Out of 766 samples analyzed, 180 samples (23.5%) contained one (131, 17.1%) or multiple (49, 6.4%) pesticides. Both the frequencies of occurrence and the rate of maximum residue level (MRL) exceedance increased in 2023 compared to 2022, with the MRL exceedance rate rising from 9.5% to 25.2%. Forty-three different residues were found in quantifiable concentrations and eight of them were non-approved. Among the residues, the non-systemic pyrethroid insecticides, lambda-cyhalothrin (8.0%) and cypermethrin (7.2%), were the two most frequently detected, with concentrations ranging from 0.010 to 0.248 mg kg-1 and from 0.011 to 0.533 mg kg-1, respectively. Turkey is a major exporter of vine leaves and these results provide crucial information regarding pesticide occurrence and quality assessment of vine leaves. The significant increase in both pesticide occurrence and MRL exceedance rates between 2022 and 2023 underscores the urgency for regulatory bodies to reassess current pesticide usage and monitoring practices. The findings emphasize the importance of implementing more stringent rules and improving enforcement methods in order to reduce the spread of unapproved pesticides and ensure adherence to global food safety standards.

Project description:New analytical approaches to the simultaneous identification and quantification of 94 pesticides and 13 polycyclic aromatic hydrocarbons (PAHs) in five representative matrices (pepper, apple, lettuce, wheat, and soil) were developed. The analyses were based on gas chromatography coupled with triple quadrupole tandem mass spectrometry (GC-MS/MS). The procedure was optimized by changing the solvent used during the extraction, from acetonitrile to the acetone: n-hexane mixture at a volume ratio of 1:4 (v/v), as well as the use of a reduced amount of water during the extraction of compounds from cereals. An additional modification was the use of florisil instead of GCB in the sample cleanup step. A full method validation study was performed, at two concentration levels (LOQ and 1000 × LOQ), which showed satisfactory results for all analytes from the PAHs group, with recoveries ranging from 70.7-115.1%, and an average RSD of 3.9%. Linearity was tested in the range of 0.001-1.000 mg/kg and showed coefficients of determination (R2) ≥ 0.99 for all PAHs. Satisfactory recovery and precision parameters (LOQ and 100 × LOQ) were achieved for almost all analytes from the pesticide group in the range of 70.1-119.3% with the mean RSD equal to 5.9%. The observed linearity for all analytes in the concentration range of 0.005-1.44 mg/kg was R2 ≥ 0.99, with the exception of famoxadone, chizalofop-p-ethyl, prothioconazole, spirodiclofen, tefluthrin, and zoxamid. The extended uncertainties were estimated, using a top-down approach of 9.9% (average) and 15.3% (average) for PAHs and pesticides samples, respectively (the coverage factor k = 2, the 95% confidence level). Ultimately, the method was successfully applied to determine pesticide residues in commercial samples of fruit, vegetables and grain, and soil samples for PAHs, which were collected from selected places in the Podkarpacie region. A total of 38 real samples were tested, in which 10 pesticides and 13 PAHs were determined. Proposed changes allow us to shorten the sample preparation time (by 20%) and to reduce the consumption of organic solvents (by 17%). The use of florisil for sample cleanup, instead of GCB, improves the recovery of compounds with flat particles.

Dataset Information

Supporting dataset on the optimization and validation of a QuEChERS-based method for the determination of 218 pesticide residues in clay loam soil.

Publications

Supporting dataset on the optimization and validation of a QuEChERS-based method for the determination of 218 pesticide residues in clay loam soil.

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