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Validation and application of a method for determination of multi-class pesticides in muscle chicken breast fillets using QuEChERS extraction and GC/MS

Aleksandra Mihail Tasic
Aleksandra Mihail Tasic
, 
Milan Ninković
Milan Ninković
 et 
Ivan Pavlović
Ivan Pavlović
   | 22 juin 2024
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Publié en ligne: 22 juin 2024
Pages: 223 - 232
Reçu: 27 nov. 2023
Accepté: 17 juin 2024
DOI: https://doi.org/10.2478/jvetres-2024-0036
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© 2024 Aleksandra Mihail Tasic et al., published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.

Fig. 1.

Full scan gas chromatography and mass spectrometry chromatograms for the analysis of multi-class pesticides in method optimisation (A) using a mixture of acetonitrile and ethyl acetate as the extraction solvent, (B) using acetonitrile as the extraction solvent
Full scan gas chromatography and mass spectrometry chromatograms for the analysis of multi-class pesticides in method optimisation (A) using a mixture of acetonitrile and ethyl acetate as the extraction solvent, (B) using acetonitrile as the extraction solvent

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
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