Validation and Simultaneous Monitoring of 311 Pesticide Residues in Loamy Sand Agricultural Soils by LC-MS/MS and GC-MS/MS, Combined with QuEChERS-Based Extraction
Abstract
:1. Introduction
2. Results
2.1. Determination of Compounds
2.1.1. Optimization of MS/MS Parameters
2.1.2. Optimization of the Extraction Efficiency
2.2. Validation of the Analytical Method
2.2.1. Method Selectivity
2.2.2. Accuracy and Precision
2.2.3. Linearity
2.2.4. Limit of Quantification and Limit of Detection
2.2.5. Matrix Effects (ME)
2.2.6. Participation in Proficiency Testing Scheme
2.3. Method Application
3. Materials and Methods
3.1. Studied Area and Sampling of Soil
3.2. Selection of Analyzed Pesticides
3.3. Analytical Methodology
3.3.1. Chemicals and Solvents
3.3.2. Standard Solutions
3.3.3. Experimental Design
3.3.4. Sample Preparation
Optimization of the Extraction Efficiency
3.3.5. Determination of Compounds—Instrumentation
Analysis of Samples with Gas Chromatography
Analysis of Samples with Liquid Chromatography
Optimization of MS/MS Parameters
3.3.6. Validation Procedure
4. Conclusions
Supplementary Materials
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Acknowledgments
Conflicts of Interest
Sample Availability
References
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Pesticide | Type | Frequency (%) | Max Concentration (mg/kg) | Approval (EC, 2022) |
---|---|---|---|---|
Azoxystrobin | F | 16 | 0.047 | Yes |
Boscalid | F | 56 | 0.11 | Yes |
Carbendazim | F | 4 | 0.037 | No |
Carfentrazon ethyl | H | 8 | 0.03 | Yes |
Clothianidin | I | 4 | 0.01 | No |
Dimethomorph | F | 20 | 1.225 | Yes |
Epoxiconazole | F | 8 | 0.01 | No |
Fludioxonil | F | 4 | 0.01 | Yes |
Fluometuron | H | 12 | 0.016 | Yes |
Imidacloprid | I | 20 | 0.024 | No |
Metconazole | F | 8 | 0.01 | Yes |
Methomyl | I | 32 | 0.147 | No |
Metolachlor | H | 4 | 0.021 | No |
Metribuzin | H | 8 | 0.015 | Yes |
Myclobutanil | F | 16 | 0.02 | No |
p,p′-DDD | I | 12 | 0.023 | No |
p,p′-DDE | I | 28 | 0.675 | No |
p,p′-DDT | I | 16 | 0.084 | No |
Penconazole | F | 32 | 0.032 | Yes |
Pendimethalin | H | 36 | 0.341 | Yes |
Pyraclostrobin | F | 4 | 0.014 | Yes |
Spinosyn A | I | 4 | 0.01 | Yes |
Tebuconazole | F | 8 | 0.025 | Yes |
Thiophanate methyl | F | 12 | 4.074 | No |
Zoxamide | F | 20 | 1.278 | Yes |
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Tsiantas, P.; Bempelou, E.; Doula, M.; Karasali, H. Validation and Simultaneous Monitoring of 311 Pesticide Residues in Loamy Sand Agricultural Soils by LC-MS/MS and GC-MS/MS, Combined with QuEChERS-Based Extraction. Molecules 2023, 28, 4268. https://doi.org/10.3390/molecules28114268
Tsiantas P, Bempelou E, Doula M, Karasali H. Validation and Simultaneous Monitoring of 311 Pesticide Residues in Loamy Sand Agricultural Soils by LC-MS/MS and GC-MS/MS, Combined with QuEChERS-Based Extraction. Molecules. 2023; 28(11):4268. https://doi.org/10.3390/molecules28114268
Chicago/Turabian StyleTsiantas, Petros, Eleftheria Bempelou, Maria Doula, and Helen Karasali. 2023. "Validation and Simultaneous Monitoring of 311 Pesticide Residues in Loamy Sand Agricultural Soils by LC-MS/MS and GC-MS/MS, Combined with QuEChERS-Based Extraction" Molecules 28, no. 11: 4268. https://doi.org/10.3390/molecules28114268