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
Soil can be contaminated by pesticide residues through agricultural practices, by direct application or through spray-drift in cultivations. The dissipation of those chemicals in the soil may pose risks to the environment and human health. A simple and sensitive multi-residue analytical method was o...
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| Format: | Article |
| Language: | English |
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MDPI AG
2023-05-01
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| Series: | Molecules |
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| Online Access: | https://www.mdpi.com/1420-3049/28/11/4268 |
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| author | Petros Tsiantas Eleftheria Bempelou Maria Doula Helen Karasali |
| author_facet | Petros Tsiantas Eleftheria Bempelou Maria Doula Helen Karasali |
| author_sort | Petros Tsiantas |
| collection | DOAJ |
| description | Soil can be contaminated by pesticide residues through agricultural practices, by direct application or through spray-drift in cultivations. The dissipation of those chemicals in the soil may pose risks to the environment and human health. A simple and sensitive multi-residue analytical method was optimized and validated for the simultaneous determination of 311 active substances of pesticides in agricultural soils. The method involves sample preparation with QuEChERS-based extraction, and determination of the analytes with a combination of GC-MS/MS and LC-MS/MS techniques. Calibration plots were linear for both detectors over the range of five concentration levels, using matrix-matched calibration standards. The obtained recoveries from fortified-soil samples ranged from 70 to 119% and from 72.6 to 119% for GC-MS/MS and LC-MS/MS, respectively, while precision values were <20% in all cases. As regards the matrix effect (ME), signal suppression was observed in the liquid chromatography (LC)-amenable compounds, which was further estimated to be negligible. The gas chromatography (GC)-amenable compounds showed enhancement in the chromatographic response estimated as medium or strong ME. The calibrated limit of quantification (LOQ) value was 0.01 μg g<sup>−1</sup> dry weight for most of the analytes, while the corresponding calculated limit of determination (LOD) value was 0.003 μg g<sup>−1</sup> d.w. The proposed method was subsequently applied to agricultural soils from Greece, and positive determinations were obtained, among which were non-authorized compounds. The results indicate that the developed multi-residue method is fit for the purpose of analyzing low levels of pesticides in soil, according to EU requirements. |
| first_indexed | 2024-03-11T03:02:09Z |
| format | Article |
| id | doaj.art-f3c21f0aed224f3bb4952f1a2839b921 |
| institution | Directory Open Access Journal |
| issn | 1420-3049 |
| language | English |
| last_indexed | 2024-03-11T03:02:09Z |
| publishDate | 2023-05-01 |
| publisher | MDPI AG |
| record_format | Article |
| series | Molecules |
| spelling | doaj.art-f3c21f0aed224f3bb4952f1a2839b9212023-11-18T08:14:19ZengMDPI AGMolecules1420-30492023-05-012811426810.3390/molecules28114268Validation and Simultaneous Monitoring of 311 Pesticide Residues in Loamy Sand Agricultural Soils by LC-MS/MS and GC-MS/MS, Combined with QuEChERS-Based ExtractionPetros Tsiantas0Eleftheria Bempelou1Maria Doula2Helen Karasali3Laboratory of Chemical Control of Pesticides, Scientific Directorate of Pesticides’ Control and Phytopharmacy, Benaki Phytopathological Institute, 8 St. Delta Str., 145 61 Kifissia, GreeceLaboratory of Chemical Control of Pesticides, Scientific Directorate of Pesticides’ Control and Phytopharmacy, Benaki Phytopathological Institute, 8 St. Delta Str., 145 61 Kifissia, GreeceLaboratory of Non-Parasitic Diseases, Scientific Directorate of Phytopathology, Benaki Phytopathological Institute, 8 St. Delta Str., 145 61 Kifissia, GreeceLaboratory of Chemical Control of Pesticides, Scientific Directorate of Pesticides’ Control and Phytopharmacy, Benaki Phytopathological Institute, 8 St. Delta Str., 145 61 Kifissia, GreeceSoil can be contaminated by pesticide residues through agricultural practices, by direct application or through spray-drift in cultivations. The dissipation of those chemicals in the soil may pose risks to the environment and human health. A simple and sensitive multi-residue analytical method was optimized and validated for the simultaneous determination of 311 active substances of pesticides in agricultural soils. The method involves sample preparation with QuEChERS-based extraction, and determination of the analytes with a combination of GC-MS/MS and LC-MS/MS techniques. Calibration plots were linear for both detectors over the range of five concentration levels, using matrix-matched calibration standards. The obtained recoveries from fortified-soil samples ranged from 70 to 119% and from 72.6 to 119% for GC-MS/MS and LC-MS/MS, respectively, while precision values were <20% in all cases. As regards the matrix effect (ME), signal suppression was observed in the liquid chromatography (LC)-amenable compounds, which was further estimated to be negligible. The gas chromatography (GC)-amenable compounds showed enhancement in the chromatographic response estimated as medium or strong ME. The calibrated limit of quantification (LOQ) value was 0.01 μg g<sup>−1</sup> dry weight for most of the analytes, while the corresponding calculated limit of determination (LOD) value was 0.003 μg g<sup>−1</sup> d.w. The proposed method was subsequently applied to agricultural soils from Greece, and positive determinations were obtained, among which were non-authorized compounds. The results indicate that the developed multi-residue method is fit for the purpose of analyzing low levels of pesticides in soil, according to EU requirements.https://www.mdpi.com/1420-3049/28/11/4268pesticide residuessoilLC-MS/MSGC-MS/MSmethod validationmulti-residue method |
| spellingShingle | Petros Tsiantas Eleftheria Bempelou Maria Doula Helen Karasali 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 pesticide residues soil LC-MS/MS GC-MS/MS method validation multi-residue method |
| title | 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 |
| title_full | 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 |
| title_fullStr | 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 |
| title_full_unstemmed | 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 |
| title_short | 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 |
| title_sort | 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 |
| topic | pesticide residues soil LC-MS/MS GC-MS/MS method validation multi-residue method |
| url | https://www.mdpi.com/1420-3049/28/11/4268 |
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