Table 3.
Accuracy and precision for antimicrobials determination in optimal UHPLC-MS/MS conditions for spiked shrimp muscle samples.
| Compound | Recovery (%) | Interday precision (RSD %) | ||||
|---|---|---|---|---|---|---|
|
|
|
|||||
| 5 ng/g | 20 ng/g | 50 ng/g | 5 ng/g | 20 ng/g | 50 ng/g | |
| Fluoroquinolones | ||||||
| ENR | 94.8 (7.9)a | 107.6 (6.0) | 98.9 (4.8) | 11.5 | 5.8 | 6.4 |
| CIP | 111.8 (8.2) | 97.3 (4.4) | 88.35 (5.4) | 16.0 | 11.5 | 11.4 |
| DIF | 106.9 (8.6) | 107.2 (5.7) | 96.2 (3.2) | 13.9 | 9.8 | 8.3 |
| SAR | 103.9 (10.0) | 93.2 (4.5) | 89.6 (4.8) | 18.1 | 6.3 | 6.8 |
| NOR | 107.1 (7.9) | 97.4 (4.6) | 91.3 (5.3) | 17.4 | 8.7 | 8.9 |
| DAN | 105.1 (10.1) | 98.1 (4.0) | 89.4 (4.5) | 18.5 | 12.7 | 14.2 |
| OFL | 109.5 (6.4) | 99.8 (4.9) | 87.3 (4.4) | 18.5 | 7.8 | 11.3 |
| GAT | 109.8 (7.4) | 103.7 (4.7) | 97.0 (6.2) | 22.7 | 8.9 | 10.6 |
| MOX | 108.9 (8.0) | 105.4 (3.5) | 97.9 (7.1) | 18.7 | 14.8 | 11.0 |
| PEF | 94.2 (10.7) | 100.1 (3.2) | 96.6 (6.7) | 20.4 | 10.6 | 17.2 |
| MAR | 104.9 (8.7) | 104.6 (3.1) | 99.8 (5.2) | 14.7 | 12.8 | 11.2 |
| FLE | 96.9 (11.2) | 103.7 (4.5) | 92.5 (5.0) | 23.0 | 8.4 | 9.7 |
| SPA | 107.8 (11.7) | 97.7 (9.5) | 87.1 (4.0) | 12.0 | 13.7 | 11.3 |
| ORB | 104.7 (9.6) | 99.8 (9.2) | 90.0 (7.3) | 19.7 | 6.6 | 7.5 |
| OXO | 113.1 (5.1) | 97.2 (9.2) | 84.7 (6.7) | 20.6 | 12.7 | 10.4 |
| FLU | 102.5 (11.3) | 106.9 (10.1) | 98.4 (6.8) | 21.1 | 12.8 | 11.0 |
| NAL | 97.6 (5.8) | 92.3 (8.3) | 82.2 (4.4) | 21.6 | 14.1 | 12.2 |
| Sulfonamides | ||||||
| SDZ | 87.5 (5.2) | 97.0 (7.5) | 94.0 (10.8) | 10.1 | 8.1 | 10.0 |
| SDMX | 77.9 (5.9) | 79.0 (4.1) | 77.8 (5.3) | 14.3 | 11.8 | 10.2 |
| SMR | 87.7 (5.1) | 103.8 (8.1) | 95.9 (11.2) | 19.7 | 7.8 | 10.0 |
| SMZ | 84.0 (6.9) | 90.5 (8.0) | 83.7 (12.7) | 14.2 | 7.6 | 8.9 |
| SMXZ | 93.3 (8.9) | 92.9 (6.4) | 90.1 (5.9) | 22.5 | 6.1 | 7.0 |
| SQX | 78.6 (5.2) | 76.7 (5.7) | 77.7 (4.5) | 17.6 | 9.9 | 10.0 |
| SCP | 84.2 (12.7) | 97.4 (4.1) | 95.3 (9.1) | 16.0 | 8.0 | 13.8 |
| SDX | 82.4 (9.0) | 89.6 (3.7) | 83.7 (5.5) | 17.4 | 8.8 | 8.5 |
| SMPZ | 74.9 (4.7) | 88.4 (7.0) | 83.1 (11.5) | 17.8 | 10.4 | 7.2 |
| SMX | 81.4 (10.0) | 86.1 (6.1) | 82.1 (11.6) | 17.4 | 7.9 | 10.7 |
| SMTZ | 83.2 (13.2) | 106.4 (8.2) | 101.9 (10.0) | 21.8 | 10.5 | 9.1 |
| SFX | 90.6 (9.7) | 99.9 (5.6) | 101.0 (3.8) | 18.1 | 16.7 | 18.9 |
| STZ | 85.6 (4.8) | 94.3 (5.3) | 93.6 (9.1) | 13.6 | 5.0 | 5.5 |
| SPZ | 85.2 (9.8) | 77.6 (5.8) | 77.8 (6.2) | 23.2 | 11.1 | 7.9 |
| SPD | 80.1 (6.1) | 93.0 (7.0) | 91.6 (10.8) | 18.1 | 8.0 | 7.8 |
| SMM | 103.3 (7.7) | 99.8 (4.4) | 95.4 (9.8) | 10.7 | 5.9 | 6.6 |
| Tetracyclines | ||||||
| OTC | 95.3 (9.6) | 91.4 (5.4) | 87.6 (5.3) | 20.4 | 14.3 | 10.3 |
| TC | 101.1 (8.3) | 102.0 (7.5) | 91.8 (6.3) | 19.9 | 8.8 | 7.3 |
| CTC | 111.0 (7.7) | 108.4 (6.7) | 104.1 (7.4) | 10.9 | 8.5 | 7.6 |
| DC | 102.1 (5.4) | 99.0 (5.1) | 94.7 (9.8) | 17.4 | 7.5 | 9.6 |
| Macrolides | ||||||
| ERY | 104.1 (10.2) | 110.6 (7.0) | 111.1 (6.3) | 15.6 | 13.4 | 14.0 |
| TIL | 105.9 (11.2) | 106.0 (4.2) | 102.1 (2.7) | 13.5 | 12.2 | 16.3 |
| TYL | 77.0 (10.4) | 74.3 (6.5) | 78.9 (8.5) | 12.0 | 11.9 | 7.9 |
| JOS | 86.2 (14.5) | 86.8 (10.4) | 89.6 (7.2) | 16.6 | 10.0 | 9.1 |
| SPI | 84.0 (11.6) | 83.2 (7.6) | 89.7 (10.6) | 18.9 | 20.8 | 12.3 |
| Lincosamides | ||||||
| LIN | 113.3 (5.0) | 112.9 (3.4) | 107.3 (4.6) | 12.4 | 7.5 | 7.7 |
| CLI | 99.2 (5.8) | 112.5 (2.9) | 108.4 (9.7) | 9.7 | 5.9 | 7.7 |
| Penicillins | ||||||
| AMP | 98.3 (7.5) | 83.0 (5.7) | 80.1 (6.8) | 11.1 | 11.0 | 10.4 |
| OXA | 93.4 (7.5) | 94.6 (4.2) | 94.9 (4.7) | 22.7 | 9.2 | 9.4 |
| DIC | 82.6 (8.6) | 88.6 (5.7) | 86.8 (3.3) | 22.0 | 16.1 | 14.8 |
| PEN G | 96.9 (5.8) | 94.8 (7.3) | 97.8 (8.4) | 18.9 | 16.4 | 14.6 |
| Nitroimidazoles b | ||||||
| DMZ | 90.8 (7.0) | 101.3 (10.5) | 96.6 (11.5) | 20.2 | 11.9 | 11.8 |
| MNZ | 86.3 (2.8) | 110.0 (4.4) | 105.3 (3.5) | 12.4 | 8.2 | 8.5 |
| RNZ | 96.8 (8.2) | 110.3 (4.9) | 104.5 (3.0) | 8.6 | 4.8 | 6.2 |
| Amphenicols c | ||||||
| FF | 110.8 (7.0) | 111.3 (6.7) | 105.5 (6.3) | 16.6 | 12.5 | 13.7 |
a
Intraday precision expressed as % RSD.
b
Evaluated at 3, 7.5 and 15 ng/g for low, medium and high concentration levels, respectively.
c
Evaluated at 10, 30 and 50 ng/g for low, medium and high concentration levels, respectively.