quadrupole; QTOF: Quadrupole time of flight; QTRAP: Hybrid triple quadrupole-linear ion trap; SBSE: Stir bar sorptive extraction; SPE: Solid phase extraction; SPME: Solid phase microextraction; TPs: Transformation products; UHPLC: Ultra-high-performance liquid chromatography; WAX: Weak anion exchange; WCX: Weak cation exchange.
bLimit of detection.
In relation to solid samples, such as soils, the most common methods were based on solid-liquid extraction (SLE), pressurized liquid extraction (PLE) and QuEChERS (see Table 1.2). In SLE methods, solvent mixtures such as acetonitrile and water have been widely used. For example, a mixture of water/acetonitrile (10 : 90, v/v) was utilized to monitor pesticide residues in soils from Argentina [62], or a mixture of water/acetonitrile (40 : 60, v/v) was used for the extraction of oxanilic and sulfonic acids metabolites [92]. Hu et al. employed methanol:water (50 : 50, v/v) instead of acetonitrile for the extraction of acetochlor and propisochlor in soils from Beijing (China) [63]. Colazzo et al. tested different solvents and mixtures, such as acetonitrile, methanol, water and methanol/water, choosing methanol as the best option (recoveries ranged from 45 to 90%) to determine pesticide residues in paddy fields and sugar cane from Uruguay [93].
Table 1.2 Overview of analytical methods applied to determine pesticides in soil matrices.a
| Pesticides | Extraction | Determination technique | Recovery (%) | LOQ (µg kg−1) | Reference |
|---|---|---|---|---|---|
| Famoxadone and metabolites | SLE: Water/Acetonitrile 1% acetic acid (50 : 50, v/v) | LC-Orbitrap-MS | 72–113 | 20 | [28] |
| OCPs, OPPs, pyrethroids (58) | SLE: Water/Acetonitrile 1% acetic acid. Extraction salts: MgSO4 and sodium acetate Clean-up: MgSO4, PSA & C18 | GC-QqQ-MS/MS | 69−119 | 100−5000 | [61] |
| 30-multicalss | SLE: Methanol Clean-up: SPE (Oasis HLB) | LC-QTRAP-MS/MS | 70−120 | 1−10 | [93] |
| 18-multiclass | SLE: Water/Acetonitrile (1 : 5, v/v) | LC-QqQ-MS/MS | 50−120 | 50 | [62] |
| Fenamidone, propamocarb | SLE: Methanol or Water Clean-up: MgSO4 & PSA | LC-QqQ-MS/MS | 77−108 | 0.4–2 | [100] |
| Oxanilic and sulfonic acid metabolites of acetochlor | SLE: Acetonitrile /Water (60 : 40, v/v) | LC-QqQ-MS/MS | 91−120 | 1−2 | [92] |
| Endosulfan, chlorpyrifos and their metabolites | SLE: Ethyl acetate with a 1 : 5 (w/v) soil-to-solvent ratio | GC-IT-MS | 76−95 | 10−50b | [29] |
| Acetochlor and Propisochlor | SLE: Methanol/water (1 : 1 v/v) Clean-up: PSA | GC-ECD | 80−116 | 10 | [63] |
| 10 OCPs | SLE: Water/Acetonitrile Clean-up: MgSO4 | GC-QqQ-MS/MS | 70−115 | 2−40 | [106] |
| 10 OCPs and metabolites | QuEChERS. Clean-up: Sulfuric acid and florisil | GC-IRMS | 60−100 | 500 | [115] |
| 218 | QuEChERS using Acetonitrile 2.5% formic acid. Extraction salts: MgSO4 & sodium acetate | LC-QqQ-MS/MS GC-QqQ-MS/MS | 70−120 | 0.5−20 | [99] |
| Pydiflumetofen enantiomers | QuEChERS Clean-up: MgSO4 & C18 | UHPLC-QqQ-MS/MS | 84–103 | 5 | [97] |
| Pyrethroid pesticide metabolite | QuEChERS Clean-up: d-SPE | GC-IT-MS | 70−94 | 13 | [64] |
| 32-multiclass | UAE: 40 mL of methanol–water (4 : 1 v/v). 20 minutes | LC-Q-MS | 60−110 | 1.5−5.0 | [107] |
| 25-Triazines, phenylureas, phenoxy acid pesticides | PLE: Dichloromethane –acetone (1 : 1, v/v) and Acetonitrile–water (2 : 1, v/v) | LC-QqQ-MS/MS | 65−120 | 0.1−3 | [95] |
| 51 Fungicides and insecticides | PLE: Methanol:acetonitrile (70 : 30, v/v) Methanol: Acetonitrile:formic acid (65 : 30:5, v/v) | LC-QqQ-MS/MS | 57−136 | 0.3−8.5 | [96] |
| 9 OPCs & PAHs | MAE: Hexane/water (3 : 2 v/v) | GC-QqQ-MS/MS | − | − | [104] |
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