Development of a Modified QuEChERS Procedure for the Isolation of Pesticide Residues from Textile Samples, Followed by GC–MS Determination
Abstract
:1. Introduction
2. Materials and Methods
2.1. Chemicals and Reagents
2.2. Sample Preparation
2.3. Instrument and Apparatus
2.4. Validation Process
3. Results
3.1. Modification of the QuEChERS Method
3.2. Sample Weight Selection
3.3. Selection of Extraction Solvent
3.4. Selection of an Appropriate Sorbent for Dispersive SPE
3.5. Method Validation
3.6. Real Sample Analysis
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Conflicts of Interest
References
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Pesticide | Retention Time [min] | Chemical Function | Fragment Ions [m/z] | Starting Time of SIM Group [min] | ||
---|---|---|---|---|---|---|
Carbofuran | 4.207 | Carbamate | 164 | 149 | 131 | 3.00 |
Trifluralin | 5.499 | Dinitroanyline | 306 | 264 | 307 | |
Hexachlorobenzene | 5.796 | OCP | 284 | 286 | 282 | 5.70 |
Dimethoate | 5.894 | OPP | 87 | 93 | 164 | |
Atrazin | 5.968 | Triazine | 200 | 215 | 202 | |
Propazin | 5.979 | Triazine | 214 | 229 | 172 | |
Diazinone | 6.025 | OPP | 179 | 137 | 152 | |
Lindane | 6.042 | OPP | 181 | 183 | 109 | |
Parathion-methyl | 6.579 | OPP | 263 | 125 | 211 | 6.30 |
Prometrin | 6.642 | Triazine | 241 | 184 | 226 | |
Fenitrothion | 6.768 | OPP | 277 | 125 | 260 | 6.74 |
Malathion | 6.808 | OPP | 173 | 127 | 125 | |
Chlorpyrifos | 6.899 | OPP | 197 | 314 | 199 | |
Parathion-ethyl | 6.977 | OPP | 291 | 109 | 139 | |
Aldrin | 6.997 | OCP | 263 | 261 | 265 | |
Dicofol | 7.117 | OCP | 139 | 111 | 250 | |
Pendimethalin | 7.242 | Dinitroanyline | 252 | 162 | 281 | 7.19 |
Oxychlordane | 7.379 | OCP | 353 | 355 | 115 | |
Heptachlor epoxide | 7.408 | OCP | 353 | 355 | 351 | |
Bromophos-ethyl | 7.557 | OPP | 359 | 357 | 303 | |
o,p-DDE | 7.642 | OCP | 246 | 248 | 318 | |
p,p-DDE | 7.997 | OCP | 246 | 318 | 316 | 7.75 |
Endosulfan-alfa | 7.808 | OCP | 241 | 239 | 195 | |
Endrin | 8.368 | OCP | 263 | 265 | 281 | 8.15 |
Endosulfan-beta | 8.471 | OCP | 237 | 239 | 216 | |
o,p-DDT | 8.500 | OCP | 235 | 237 | 165 | |
p,p-DDT | 8.883 | OCP | 235 | 237 | 165 | 8.80 |
Endosulfan sulfate | 8.923 | OCP | 229 | 272 | 387 | |
Bifenthrin | 9.243 | Pyrethroid | 181 | 165 | 166 | |
Methoxychlor | 9.391 | OCP | 227 | 228 | 274 | |
Cyhalothrin lambda | 9.746 | Pyrethroid | 181 | 197 | 208 | 9.56 |
Cypermethrin | 10.797 | Pyrethroid | 163 | 165 | 181 | |
Deltamethrin | 11.952 | Pyrethroid | 181 | 253 | 251 |
Name | ER% 10 µg/kg (RSD%) | ER% 50 µg/kg (RSD%) | ER% 250 µg/kg (RSD%) | LCL [µg/kg] | LOD [µg/kg] | LOQ [µg/kg] | MRL [µg/kg] |
---|---|---|---|---|---|---|---|
Carbofuran | 88 (6) | 91 (4) | 92 (2) | 5 | 0.980 | 3.240 | 100 |
Trifluralin | 101 (2) | 86 (6) | 95 (1) | 0.5 | 0.057 | 0.190 | 10 |
Hexachlorobenzene | 96 (7) | 97 (1) | 104 (1) | 5 | 0.750 | 2.470 | 20 |
Dimethoate | 62 (13) | 96 (11) | 94 (7) | 5 | 1.400 | 4.620 | 10 |
Atrazine | 97 (6) | 96 (4) | 102 (1) | 5 | 1.210 | 3.980 | 50 |
Propazin | 98 (4) | 94 (3) | 101 (2) | 0.1 | 0.090 | 0.290 | |
Diazinon | 100 (4) | 102 (9) | 101 (2) | 5 | 1.402 | 4.673 | 20 |
Lindane | 70 (10) | 97 (9) | 95 (7) | 5 | 1.490 | 4.910 | 10 |
Parathion methyl | 63 (13) | 90 (9) | 92 (7) | 5 | 1.360 | 4.500 | 20 |
Promethryn | 100 (2) | 97 (3) | 101 (2) | 0.1 | 0.060 | 0.190 | |
Fenitrothion | 70 (15) | 97 (9) | 88 (9) | 5 | 1.500 | 4.950 | 20 |
Malathion | 64 (9) | 95 (8) | 90 (9) | 5 | 1.520 | 5.000 | 20 |
Chlorpyrifos | 101 (3) | 101 (3) | 104 (1) | 0.1 | 0.060 | 0.190 | 300 |
Parathion ethyl | 99 (2) | 98 (6) | 104 (2) | 1 | 0.149 | 0.495 | |
Aldrin | 98 (3) | 95 (5) | 104 (1) | 5 | 0.980 | 3.240 | 20 |
Dicofol | 122 (11) | 103 (9) | 92 (9) | 5 | 1.520 | 5.000 | 100 |
Pendimethalin | 96 (5) | 92 (5) | 101 (4) | 5 | 1.320 | 4.350 | 50 |
Oxychlordan | 98 (4) | 96 (2) | 102 (1) | 0.5 | 0.366 | 1.220 | |
Heptachlorepoxid | 100 (1) | 96 (1) | 103 (2) | 0.5 | 0.366 | 1.220 | 10 |
Bromophos ethyl | 101 (1) | 96 (2) | 104 (1) | 0.1 | 0.045 | 0.149 | 20 |
O,p-DDE | 98 (3) | 97 (6) | 105 (2) | 0.1 | 0.035 | 0.118 | 50 |
Endosulfan alfa | 70 (8) | 92 (4) | 100 (3) | 5 | 1.130 | 3.740 | 30 |
P,p-DDE | 97 (1) | 95 (4) | 104 (1) | 0.5 | 0.161 | 0.538 | 50 |
Endrin | 75 (9) | 96 (2) | 103 (1) | 5 | 1.390 | 4.600 | |
Endosulfan beta | 100 (2) | 106 (5) | 101 (2) | 5 | 1.290 | 4.250 | 30 |
O,p-DDT | 102 (3) | 98 (5) | 100 (6) | 5 | 1.260 | 4.170 | 50 |
P,p-DDT | 99 (1) | 106 (10) | 96 (7) | 5 | 0.843 | 2.809 | 50 |
Endosulfan sulfat | 72 (14) | 89 (13) | 97 (8) | 5 | 1.520 | 5.000 | 30 |
Bifenthrin | 99 (1) | 95 (1) | 105 (1) | 0.5 | 0.128 | 0.427 | 500 |
Methoxychlor | 94 (11) | 95 (15) | 99 (13) | 0.1 | 0.030 | 0.090 | 10 |
Cyhalotrin lambda | 98 (3) | 95 (8) | 93 (8) | 1 | 0.280 | 0.910 | 200 |
Cypermethrin | 96 (2) | 99 (7) | 93 (7) | 1 | 0.260 | 0.850 | 200 |
Deltamethrin | 100 (4) | 102 (8) | 91 (5) | 1 | 0.270 | 0.900 | 20 |
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Hrouzková, S.; Szarka, A. Development of a Modified QuEChERS Procedure for the Isolation of Pesticide Residues from Textile Samples, Followed by GC–MS Determination. Separations 2021, 8, 106. https://doi.org/10.3390/separations8080106
Hrouzková S, Szarka A. Development of a Modified QuEChERS Procedure for the Isolation of Pesticide Residues from Textile Samples, Followed by GC–MS Determination. Separations. 2021; 8(8):106. https://doi.org/10.3390/separations8080106
Chicago/Turabian StyleHrouzková, Svetlana, and Agneša Szarka. 2021. "Development of a Modified QuEChERS Procedure for the Isolation of Pesticide Residues from Textile Samples, Followed by GC–MS Determination" Separations 8, no. 8: 106. https://doi.org/10.3390/separations8080106