Fig. 1.
List of pesticide residues and definitions, chemical classification and action (25), retention time, quantifier and qualifier ions, calibration curves, correlation coefficients and linearity (range 5–50 μg/kg)
| Analyte | Chemical class | Pesticide action | Retention time, min | Quantifier trace | Qualifier ion, 1 > 2 > 3 | Calibration curve | R2 |
|---|---|---|---|---|---|---|---|
| Dichlorvos | Organophosphate | IN | 5.58 | 109 | 185 >79 >187 | y=3.233x + 16.244 | 0.998759 |
| Acephate | Organophosphate | IN | 7.47 | 136 | 94 >42 >95 | y=0.611x − 55.278 | 0.994125 |
| Propoxur | Carbamate | IN | 9.96 | 110 | 152 >57 >111 | y=0.516x − 0.659 | 0.999237 |
| Ethoprophos | Organophosphate | IN, NE | 10.41 | 158 | 97 >126 >139 | y=0.678x−10.689 | 0.997375 |
| α-HCH | Organochlorine | IN | 11.74 | 181 | 183 > 219>217 | y=0.821x + 0.192 | 0.997180 |
| Dimethoate | Organophosphate | IN | 12.34 | 87 | 93 > 125 >143 | y=1.450x − 46.247 | 0.995620 |
| Carbofuran | Carbamate | IN, NE, AC | 12.59 | 164 | 149 >131 >123 | y=1.376x − 23.924 | 0.999150 |
| β-HCH | Organochlorine | IN | 13.09 | 219 | 181 >183 >217 | y=1.303x + 8.942 | 0.996873 |
| Lindan | Organochlorine | IN | 13.14 | 181 | 183 >219 >111 | y=1.206x + 13.008 | 0.998267 |
| Diazinon | Organophosphate | IN | 13.78 | 179 | 137 >152 >199 | y=0.739x − 4.005 | 0.999704 |
| δ-HCH | Organochlorine | IN | 14.65 | 181 | 219 >183 >217 | y=0.603x + 1.174 | 0.997564 |
| Methyl parathion | Organophosphate | IN | 16.28 | 263 | 109 >125 >79 | y=0.613x − 18.484 | 0.998040 |
| Spiroxamine I | Morpholine | FU | 16.33 | 100 | 101 >126 >198 | y=0.134x + 1.758 | 0.997711 |
| Heptachlor | Organochlorine | IN | 16.49 | 100 | 270 >272 >274 | y=0.694x + 14.471 | 0.994716 |
| Carbaryl | Carbamate | IN, PG | 16.66 | 144 | 115 >116 >145 | y=1.701x − 60.691 | 0.990595 |
| Metalaxyl | Phenylamide | FU | 16.77 | 206 | 45 >160 >249 | y=1.444x − 18.488 | 0.998995 |
| Aldrin | Organochlorine | IN | 18.45 | 100 | 101 >126 >198 | y=0.948x + 12.281 | 0.996261 |
| Malathion | Organophosphate | IN | 18.26 | 173 | 127 >125 >93 | y=0.898x − 21.530 | 0.999616 |
| Spiroxamine II | Morpholine | FU | 18.23 | 263 | 66 >265 >261 | y=0.705x − 10.898 | 0.999415 |
| Chlorpyrifos | Organophosphate | IN | 18.46 | 197 | 199 >314 >97 | y=0.908x − 16.933 | 0.998991 |
| Heptachlor epoxide (trans, isomer A) | Organochlorine | IN | 20.70 | 351 | 353 >355 >357 | y=0.344x + 2.547 | 0.991486 |
| Fipronil | Aminopyrazole carbonitrile | IN | 21.13 | 367 | 369 >213 >351 | y=0.437x − 17.073 | 0.997170 |
| trans Chlordane | Organochlorine | IN | 21.79 | 373 | 375 >377 >371 | y=0.462x − 2.332 | 0.998275 |
| Prallethrin cis | Pyrethroid | IN | 22.17 | 123 | 105 >81 >134 | y=0.350x − 15.113 | 0.993093 |
| Prallethrin trans | Pyrethroid | IN | 22.24 | 123 | 81 >105 >77 | y=0.416x − 20.457 | 0.998616 |
| Paclobutrazol | Triazole | PG | 22.40 | 236 | 125 >238 >167 | y=0.761x − 44.487 | 0.993356 |
| α-Endosulfan | Organochlorine | IN | 22.43 | 241 | 195 >239 >238 | y=0.213x + 0.518 | 0.996908 |
| cis Chlordane | Organochlorine | IN | 22.47 | 373 | 375 >377 >371 | y=0.473x − 6.305 | 0.996973 |
| Imazalil | Imidazole | FU | 23.40 | 41 | 215 >173 >217 | y=0.665x − 10.165 | 0.994770 |
| Fludioxonil | Phenylpyrrole | FU | 23.85 | 248 | 127 >154 >182 | y=0.517x − 23.688 | 0.993647 |
| Dieldrin | Organochlorine | IN | 23.72 | 79 | 263 >277 >279 | y=1.184x + 0.013 | 0.999207 |
| p, p′-DDE | Organochlorine metabolite | IN | 23.77 | 246 | 318 >316 >248 | y=1.613x − 67.643 | 0.999926 |
| Kresoxim methyl | Strobilurin | FU | 24.36 | 116 | 206 >131 >132 | y=1.645x − 28.114 | 0.998792 |
| Chlorfenapyr | Halogenated pyrrole | IN | 24.68 | 59 | 247 >249 >408 | y=0.478x + 2.522 | 0.999517 |
| Endrin | Organochlorine | IN | 24.60 | 263 | 317 >265 >245 | y=0.479x − 1.059 | 0.991602 |
| Beta Endosulfan | Organochlorine | IN | 25.09 | 195 | 237 >207 >241 | y=0.572x − 0.110 | 0.998883 |
| p, p′-DDD | Organochlorine metabolite | IN | 25.49 | 235 | 237 >165 >236 | y=1.940x − 14.977 | 0.998987 |
| Endosulfan sulphate | Organochlorine metabolite | IN | 26.53 | 272 | 274 >229 >237 | y=0.263x − 4.496 | 0.998369 |
| Propiconazole I | Triazole | FU | 26.60 | 69 | 173 >259 >175 | y=0.743x − 10.101 | 0.998569 |
| Trifloxystrobin | Strobilurin | FU | 26.73 | 116 | 131 >59 >172 | y=1.265x − 37.722 | 0.998671 |
| Propiconazole II | Triazole | FU | 26.79 | 173 | 69 >259 >175 | y=1.098x − 14.776 | 0.998890 |
| p, p′-DDT | Organochlorine metabolite | IN | 26.77 | 235 | 237 >165 >236 | y=1.313x − 25.359 | 0.999525 |
| Tebuconazole | Triazole | FU | 27.28 | 125 | 250 >70 >83 | y=1.104x − 33.413 | 0.999160 |
| Spiromesifen | Spirocyclic tetronic acid | IN | 27.83 | 272 | 99 > 273 > 254 | y=0.266x − 5.603 | 0.992335 |
| Endrin ketone | Organochlorine metabolite | IN | 28.00 | 317 | 67 >315 >319 | y=0.262x + 0.423 | 0.999700 |
| Phosmet | Organophosphate | IN | 28.24 | 160 | 161 >77 >93 | y=3.378x − 136.602 | 0.992964 |
| Bifenthrin | Pyrethroid | IN | 28.43 | 181 | 165 >166 >182 | y=3.946x − 43.476 | 0.999588 |
| Fenoxycarb | Carbamate | IN | 28.56 | 255 | 186 >77 >185 | y=0.641x − 11.790 | 0.990529 |
| Methoxychlor | Organochlorine | IN | 28.60 | 113 | 152 >227 >228 | y=2.679x − 69.052 | 0.999788 |
| Etoxazole | Diphenyloxazole | AC | 28.64 | 141 | 204 >300 >359 | y=0.268x + 0.366 | 0.999849 |
| Permethrin I | Pyrethroid | IN | 31.04 | 183 | 163 >165 >184 | y=2.405x + 0.438 | 0.999773 |
| Pyridaben | Pyridazinone | IN, AC | 31.24 | 147 | 117 >148 >132 | y=3.412x − 41.245 | 0.998908 |
| Permethrin II | Pyrethroid | IN | 31.23 | 183 | 163 >165 >184 | y=2.228x − 12.107 | 0.999740 |
| Cyfluthrin I | Pyrethroid | IN | 31.84 | 163 | 206 >165 >226 | y=0.175x + 0.333 | 0.999504 |
| Cyfluthrin II | Pyrethroid | IN | 31.99 | 163 | 206 >165 >226 | y=0.222x + 2.497 | 0.994932 |
| Cyfluthrin III | Pyrethroid | IN | 32.06 | 163 | 206 >165 >226 | y=0.246x − 6.336 | 0.998605 |
| Cyfluthrin IV | Pyrethroid | IN | 32.13 | 163 | 206 >165 >226 | y=0.124x + 4.731 | 0.995465 |
| Cypermethrin I | Pyrethroid | IN | 32.31 | 181 | 163 >165 >209 | y=0.182x + 1.980 | 0.998705 |
| Cypermethrin II | Pyrethroid | IN | 32.45 | 181 | 163 >165 >209 | y=0.250x − 1.053 | 0.995146 |
| Cypermethrin III | Pyrethroid | IN | 32.54 | 181 | 163 >165 >209 | y=0.139x − 0.982 | 0.994351 |
| Cypermethrin IV | Pyrethroid | IN | 32.63 | 181 | 163 >165 >209 | y=0.147x − 1.307 | 0.999349 |
| Boscalid | Carboxamide/anilide | FU | 32.40 | 140 | 342 >344 >142 | y=2.222x − 23.456 | 0.997997 |
| Etofenprox | Pyrethroid | IN | 32.75 | 163 | 164 >135 >107 | y=4.654x + 51.022 | 0.999801 |
| Azoxystrobin | Strobilurin | FU | 35.68 | 344 | 388 >345 >372 | y=0.956x − 3.589 | 0.999298 |
Pesticides detected and their concentrations in chicken breast fillets
| Sample | Number of samples, pesticide <LOQ | Number of samples, pesticide, >LOQ | Cypermethrin (sum of isomers – μg/kg) | Endosulfan sulphate, (μg/kg) | Permethrin, (sum of isomers) μg/kg | Alpha endosulfan, μg/kg | p,p′-DDT, μg/kg |
|---|---|---|---|---|---|---|---|
| Domestic chicken fillets | 37 | 3 | <LOQ–11.5 | <LOQ–4.9 | <LOQ–15.2 | <LOQ -5.4 | <LOQ |
| Imported chicken fillets | 39 | 1 | <LOQ | <LOQ | <LOQ | <LOQ | <LOQ–6.0 |
| Organic domestic chicken fillets | 20 | 0 | <LOQ | <LOQ | <LOQ | <LOQ | <LOQ |
| Calculated value using Cf | / | / | 11.5 | 4.7 | 15.2 | 5.4 | 6.0 |
| MRL (sum) | / | / | 100 | 50 | 50 | 50 | 1000 |
Recovery, relative standard deviation (RSD), limit of detection (LOD) and limit of quantification (LOQ) for determination of multi-class pesticides
| No. | Pesticide | Recovery (RSD), % (n = 6) 5 μg/kg | Recovery (RSD), % (n = 6) 10 μg/kg | Recovery (RSD), % (n = 6) 20 μg/kg | LOD (n = 6) μg/kg | LOQ (n = 6) μg/kg |
|---|---|---|---|---|---|---|
| 1 | Acephate | 72.8 (9.2) | 71.8 (9.1) | 84.2 (14.9) | 1.1 | 3.6 |
| 2 | Aldrin | 75.2 (11.2) | 78.2 (10.0) | 105.2 (9.8) | 1.3 | 4.2 |
| 3 | α-Endosulfan | 83.2 (6.5) | 79.4 (7.0) | 84.0 (9.8) | 1.2 | 4.0 |
| 4 | α-HCH | 81.2 (6.1) | 79.6 (9.4) | 77.4 (6.3) | 1.4 | 4.5 |
| 5 | Azoxystrobin | 100.5 (3.6) | 103 (13.3) | 82.1 (10.2) | 1.0 | 3.3 |
| 6 | β-Endosulfan | 88.2 (4.2) | 87.6 (13.3) | 82.1 (10.2) | 1.2 | 4.1 |
| 7 | β-HCH | 102.4 (11.3) | 114.2 (14.4) | 110.0 (14.8) | 1.2 | 4.0 |
| 8 | Bifenthrin | 92.3 (8.2) | 94.8 (10.9) | 80.8 (11.3) | 1.2 | 3.9 |
| 9 | Boscalid | 102.3 (4.6) | 109.0 (10.9) | 95.6 (10.7) | 1.1 | 3.7 |
| 10 | Carbaryl | 102.4 (3.8) | 95.6 (8.9) | 106.2 (16.2) | 1.5 | 4.9 |
| 11 | Carbofuran | 86.9 (11.9) | 83.8 (13.6) | 84.0 (10.1) | 1.4 | 4.8 |
| 12 | Chlorfenapyr | 79.5 (5.2) | 71.2 (11.7) | 82.4 (12.6) | 1.6 | 5.2 |
| 13 | Chlorpyrifos | 99.4 (3.2) | 97.0 (6.1) | 84.6 (12.0) | 1.4 | 4.5 |
| 14 | cis-Chlordane | 90.7 (6.3) | 90.8 (12.7) | 92.0 (14.2) | 1.4 | 4.5 |
| 15 | Cyfluthrin (sum) | 112.5 (7.2) | 114.1 (12.9) | 117.2 (7.8) | 0.9 | 3.1 |
| 16 | Cypermethrin (sum) | 99.5 (3.5) | 110.0 (9.6) | 84.4 (15.5) | 1.2 | 4.0 |
| 17 | δ-HCH | 93.4 (9.2) | 89.8 (10.3) | 110.2 (11.7) | 1.1 | 3.7 |
| 18 | Diazinon | 99.9 (8.1) | 96.3 (11.4) | 105.8 (1.7) | 1.4 | 4.6 |
| 19 | Dichlorvos | 83.2 (12.4) | 82.2 (14.9) | 83.2 (12.7) | 1.5 | 4.9 |
| 20 | Dieldrin | 105.6 (4.5) | 107.2 (6.2) | 113.0 (14.3) | 0.9 | 3.1 |
| 21 | Dimethoate | 111.1 (4.3) | 112.2 (7.2) | 112.6 (4.5) | 1.0 | 3.2 |
| 22 | Endosulfan sulphate | 98.5 (5.8) | 114.4 (4.1) | 102.2 (8.3) | 0.9 | 3.1 |
| 23 | Endrin | 87.8 (8.2) | 82.8 (13.6) | 73.6 (7.5) | 1.0 | 3.5 |
| 24 | Endrin ketone | 82.5 (3.6) | 81.0 (13.8) | 101.6 (2.9) | 1.0 | 3.4 |
| 25 | Etofenprox | 99.9 (11.6) | 102.0 (18.9) | 95.5 (13.2) | 1.0 | 3.5 |
| 26 | Ethoprophos | 94.6 (5.7) | 104.0 (7.8) | 87.8 (14.3) | 1.4 | 4.8 |
| 27 | Etoxazole | 111.6 (14.2) | 118.8 (12.5) | 113.0 (12.5) | 1.4 | 4.7 |
| 28 | Fenoxycarb | 89.2 (7.8) | 77.2 (13.5) | 81.8 (17.8) | 1.4 | 4.5 |
| 29 | Fipronil | 106.3 (12.4) | 104.6 (17.4) | 86.8 (17.9) | 0.9 | 3.0 |
| 30 | Fipronil sulfone | 103.1 (3.5) | 102.1 (6.3) | 109.4 (4.9) | 0.9 | 3.0 |
| 31 | Fludioxonil | 86.3 (4.9) | 89.4 (4.6) | 80.0 (18.1) | 1.2 | 4.0 |
| 32 | Heptachlor | 85.4 (4.1) | 80.2 (4.1) | 86.0 (8.5) | 1.2 | 4.0 |
| 33 | Heptachlor epoxide (trans-, isomer A) | 98.7 (4.4) | 89.6 (11.8) | 99.8 (15.2) | 1.4 | 4.8 |
| 34 | Imazalil | 99.8 (12.3) | 97.4 (16.6) | 102 (18.0) | 0.9 | 3.1 |
| 35 | Kresoxim methyl | 94.4 (2.9) | 89.2 (7.8) | 98.0 (3.6) | 1.0 | 3.4 |
| 36 | Lindane | 79.3 (6.1) | 77.4 (7.7) | 75.4 (15.1) | 1.2 | 4.0 |
| 37 | Malathion | 84.6 (6.9) | 79.4 (15.4) | 76.2 (8.1) | 1.4 | 4.6 |
| 38 | Metalaxyl | 90.2 (4.3) | 90.8 (11.5) | 106.0 (7.6) | 1.4 | 4.6 |
| 39 | Methyl parathion | 84.1 (6.7) | 83.8 (13.8) | 84.5 (6.1) | 1.4 | 4.6 |
| 40 | Metoxychlor | 74.7 (4.2) | 74.8 (6.8) | 101.2 (16.7) | 0.9 | 3.1 |
| 41 | o,p′-DDT | 92.6 (3.9) | 95.6 (3.3) | 97.9 (3.7) | 1.2 | 4.0 |
| 42 | p,p′-DDD (TDE) | 100.1 (2.9) | 89.4 (7.0) | 101.2 (16.7) | 1.2 | 4.0 |
| 43 | p,p′-DDE | 94.1 (1.6) | 93.5 (3.5) | 95.8 (11.8) | 1.0 | 3.5 |
| 44 | p,p′-DDT | 94.2 (3.0) | 84.8 (12.1) | 101.0 (13.5) | 1.0 | 3.5 |
| 45 | Paclobutrazol | 87.7 (3.5) | 79.8 (5.7) | 88.0 (13.7) | 1.4 | 4.6 |
| 46 | Permethrin (sum) | 86.6 (8.9) | 83.8 (14.8) | 102.2 (8.4) | 1.0 | 3.5 |
| 47 | Phosmet | 103.1 (2.9) | 95.2 (14.1) | 106.6 (10.6) | 1.5 | 4.9 |
| 48 | Prallethrin (sum) | 98.5 (5.5) | 102.4 (17.8) | 92.6 (5.7) | 1.0 | 3.3 |
| 49 | Propiconazole (sum) | 101.4 (11.3) | 96.0 (10.6) | 104.8 (14.4) | 1.4 | 4.6 |
| 50 | Propoxur | 75.3 (3.1) | 87.4 (10.9) | 75.2 (9.7) | 1.2 | 4.0 |
| 51 | Pyridaben | 110.3 (3.3) | 114.0 (8.1) | 85.4 (12.3) | 1.4 | 4.8 |
| 52 | Spiromesifen | 89.9 (9.9) | 81.6 (14.1) | 90.8 (10.0) | 1.2 | 4.0 |
| 53 | Spiroxamine (sum) | 113.4 (14.7) | 118.8 (10.8) | 105.4 (9.9) | 1.4 | 4.6 |
| 54 | Tebuconazole | 94.2 (7.1) | 110.6 (6.4) | 71.2 (11.1) | 1.2 | 4.0 |
| 55 | trans-Chlordane | 91.2 (4.6) | 86.0 (10.3) | 107.8 (17.2) | 1.4 | 4.6 |
| 56 | Trifloxystrobin | 104.2 (2.9) | 107.0 (15.1) | 87.2 (3.0) | 1.2 | 4.0 |