New method of analysis of nitrofurans and nitrofuran metabolites in different biological matrices using UHPLC-MS/MS
, , y | 07 jul 2018
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Publicado en línea: 07 jul 2018
Páginas: 161 - 166
Recibido: 21 feb 2018
Aceptado: 11 jun 2018
DOI: https://doi.org/10.2478/jvetres-2018-0025
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© 2018 Tomasz Śniegocki et al., published by Sciendo
This work is licensed under the Creative Commons Attribution-NonCommercial-NoDerivatives 3.0 License.
Fig. 1
Fig. 2
Validation report for nitrofuran metabolites
| Matrix | Repeatability (RSDr,%) | Within-lab reproducibility (RSDwR,%) | CCα (μg kg−1) | CCβ (μg kg−1) | Apparent recovery (%) | Matrix effect (%) | Expanded uncertainty −1(μg kg) |
|---|---|---|---|---|---|---|---|
| AOZ | |||||||
| feed water | 4.4 ± 3.4 | 5.6 ± 4.1 | 0.50 | 0.52 | 104.5 ± 2.8 | 4.0 ± 1.9% | 1.0 ± 0.14 |
| feed | 4.9 ± 4.4 | 6.6 ± 4.3 | 0.50 | 0.54 | 103.5 ± 6.8 | 6.1 ± 2.9% | 1.0 ± 0.24 |
| urine | 5.0 ± 3.7 | 6.3 ± 4.4 | 0.50 | 0.56 | 104.0 ± 4.2 | 6.0 ± 2.7% | 1.0 ± 0.2 |
| plasma | 3.1 ± 3.6 | 5.7 ± 3.2 | 0.50 | 0.52 | 98.0 ± 3.8 | 4.5 ± 3.5% | 1.0 ± 0.23 |
| muscle | 2.9 ± 4.5 | 4.5 ± 3.6 | 0.50 | 0.54 | 103.1 ± 4.2 | 5.4 ± 5.5% | 1.0 ± 0.18 |
| eggs | 7.4 ± 6.1 | 10.7 ± 6.5 | 0.50 | 0.53 | 97.0 ± 0.3 | 7.0 ± 2.5% | 1.0 ± 0.25 |
| milk | 3.2 ± 3.8 | 4.8 ± 4.4 | 0.50 | 0.54 | 96.0 ± 4.9 | 6.4 ± 4.3% | 1.0 ± 0.18 |
| honey | 6.1 ± 3.9 | 8.7 ± 5.7 | 0.50 | 0.53 | 98.7 ± 6.3 | 7.3 ± 5.5% | 1.0 ± 0.28 |
| AMOZ | |||||||
| feed water | 4.1 ± 3.4 | 6.6 ± 3.1 | 0.50 | 0.53 | 89.5 ± 3.8 | 4.0 ± 2.0% | 1.0 ± 0.18 |
| feed | 5.1 ± 5.1 | 5.3 ± 3.4 | 0.50 | 0.54 | 96.5 ± 6.8 | 6.3 ± 4.0% | 1.0 ± 0.26 |
| urine | 6.2 ± 3.9 | 7.3 ± 4.1 | 0.50 | 0.53 | 103.0 ± 4.1 | 6.3 ± 5.2% | 1.0 ± 0.15 |
| plasma | 3.6 ± 3.9 | 4.4 ± 4.2 | 0.50 | 0.53 | 95.0 ± 4.5 | 4.5 ± 5.5% | 1.0 ± 0.23 |
| muscle | 5.9 ± 3.5 | 6.4 ± 3.6 | 0.50 | 0.52 | 106.2 ± 4.1 | 5.3 ± 3.6% | 1.0 ± 0.16 |
| eggs | 5.4 ± 4.2 | 5.7 ± 6.5 | 0.50 | 0.53 | 97.2 ± 5.3 | 5.0 ± 4.5% | 1.0 ± 0.25 |
| milk | 4.2 ± 3.9 | 5.8 ± 4.4 | 0.50 | 0.52 | 105.2 ± 3.9 | 4.0 ± 4.3% | 1.0 ± 0.16 |
| honey | 5.9 ± 4.8 | 7.7 ± 4.7 | 0.50 | 0.53 | 95.7 ± 5.3 | 8.0 ± 4.5% | 1.0 ± 0.28 |
| SEM | |||||||
| feed water | 4.2 ± 2.4 | 8.4 ± 4.1 | 0.50 | 0.54 | 88.9 ± 3.8 | 3.0 ± 1.0% | 1.0 ± 0.19 |
| feed | 9.4 ± 5.4 | 8.4 ± 5.2 | 0.50 | 0.55 | 93.3 ± 5.6 | 6.3 ± 5.5% | 1.0 ± 0.35 |
| urine | 8.6 ± 4.6 | 8.4 ± 4.3 | 0.50 | 0.53 | 102.0 ± 6.3 | 6.3 ± 5.1% | 1.0 ± 0.25 |
| plasma | 4.1 ± 3.9 | 5.7 ± 4.6 | 0.50 | 0.53 | 92.0 ± 4.3 | 6.5 ± 4.5% | 1.0 ± 0.24 |
| muscle | 3.9 ± 3.5 | 5.4 ± 4.6 | 0.50 | 0.54 | 107.3 ± 5.1 | 5.3 ± 5.2% | 1.0 ± 0.26 |
| eggs | 7.4 ± 6.1 | 10.6 ± 6.8 | 0.50 | 0.55 | 97.0 ± 5.3 | 9.0 ± 4.5% | 1.0 ± 0.25 |
| milk | 5.1 ± 3.2 | 6.8 ± 5.4 | 0.50 | 0.54 | 95.0 ± 3.9 | 7.0 ± 3.5% | 1.0 ± 0.26 |
| honey | 7.0 ± 5.8 | 8.4 ± 5.7 | 0.50 | 0.55 | 95.7 ± 6.3 | 10.0 ±4.6% | 1.0 ± 0.31 |
| AHD | |||||||
| feed water | 4.9 ± 3.4 | 7.4 ± 4.1 | 0.50 | 0.54 | 100.5 ± 2.8 | 5.2 ± 2.0% | 1.0 ± 0.23 |
| feed | 5.2 ± 3.7 | 8.4 ± 6.4 | 0.50 | 0.54 | 94.9 ± 6.8 | 5.0 ± 4.3% | 1.0 ± 0.32 |
| urine | 8.2 ± 5.7 | 7.5 ± 5.5 | 0.50 | 0.52 | 106.2 ± 53 | 6.3 ± 4.6% | 1.0 ± 0.25 |
| plasma | 4.3 ± 3.4 | 4.3 ± 3.9 | 0.50 | 0.53 | 95.0 ± 5.8 | 6.7 ± 4.7% | 1.0 ± 0.28 |
| muscle | 3.9 ± 3.2 | 4.4 ± 3.9 | 0.50 | 0.53 | 102.1 ± 4.3 | 5.3 ± 5.5% | 1.0 ± 0.23 |
| eggs | 6.3 ± 5.2 | 8.7 ± 4.5 | 0.50 | 0.54 | 94.3 ± 5.3 | 4.0 ± 5.5% | 1.0 ± 0.25 |
| milk | 5.1 ± 3.3 | 6.8 ± 5.4 | 0.50 | 0.53 | 95.0 ± 6.9 | 5.2 ± 4.3% | 1.0 ± 0.28 |
| honey | 7.3 ± 4.3 | 8.1 ± 5.1 | 0.50 | 0.55 | 93.4 ± 7.3 | 10.2 ± 5.5% | 1.0 ± 0.32 |
Precursor ions and product ion transitions of nitrofuran metabolites and internal standards – mass spectrometry parameters
| Analyte | Precursor ion (m/z) | Ion transition | Declustering potential | Collision energy (eV) |
|---|---|---|---|---|
| AOZ | 235.95 | 134.0 104.0 | 116 | 15 29 |
| AMOZ | 335.00 | 291.0 262.1 | 71 | 16 26 |
| SEM | 209.00 | 166.0 192.0 | 96 | 13 15 |
| AHD | 249.00 | 134.0 104.0 | 126 | 15 27 |
| AOZ-D4 (IS) | 239.95 | 134.0 | 136 | 17 |
| AMOZ-D5 (IS) | 340.00 | 296.1 | 106 | 15 |
| SEM-C13, 2N15 (IS) | 212.00 | 167.9 | 86 | 13 |