Table 1.
Method validation data for mycotoxin determination in natural grass samples
| Analyte | Linear range (μg kg−1) | Linearity, R2 | LOD (μg kg−1) | LOQ (μg kg−1) |
|---|---|---|---|---|
| DON | 92–750 | 0.990 | 27 | 92 |
| AFG2 | 1.7–100 | 0.989 | 0.51 | 1.7 |
| AFG1 | 0.95–100 | 0.998 | 0.28 | 0.95 |
| AFB2 | 1.3–100 | 0.996 | 0.38 | 1.3 |
| AFB1 | 0.61–100 | 0.998 | 0.18 | 0.61 |
| HT-2 | 37–750 | 0.994 | 11 | 37 |
| T-2 | 17–750 | 0.995 | 5.3 | 17 |
| OTA | 1.9–100 | 0.985 | 0.57 | 1.9 |
| ENNB | 0.07–100 | 0.993 | 0.02 | 0.07 |
| BEA | 0.09–100 | 0.994 | 0.03 | 0.09 |
| ENNB1 | 0.09–100 | 0.997 | 0.03 | 0.09 |
| ENNA1 | 0.07–100 | 0.987 | 0.02 | 0.07 |
| ENNA | 0.08–100 | 0.996 | 0.02 | 0.08 |
| Trueness, % RSD (n = 9) | SSE (%) | |||
| Low level | High level | |||
| DON | 90 (4.2) | 98 (5.9) | 42.0 | |
| AFG2 | 96 (2.1) | 97 (5.3) | 52.4 | |
| AFG1 | 110 (5.9) | 100 (2.8) | 57.7 | |
| AFB2 | 90 (4.4) | 105 (5.8) | 56.4 | |
| AFB1 | 108 (6.5) | 110 (2.1) | 59.9 | |
| HT-2 | 82 (7.1) | 106 (1.9) | 66.3 | |
| T-2 | 76 (2.8) | 92 (8.7) | 47.1 | |
| OTA | 78 (2.7) | 103 (8.1) | 42.4 | |
| ENNB | 107 (4.5) | 106 (1.8) | 91.9 | |
| BEA | 95 (5.3) | 97 (1.9) | 89.6 | |
| ENNB1 | 102 (4.7) | 104 (6.1) | 92.2 | |
| ENNA1 | 99 (3.1) | 104 (2.6) | 89.5 | |
| ENNA | 104 (5.0) | 108 (3.2) | 88.0 | |
| Repeatability, % RSD (n = 6) | Intermediate precision, % RSD (n = 18) | |||
| Low level | High level | Low level | High level | |
| DON | 5.4 | 3.7 | 7.3 | 6 |
| AFG2 | 1.5 | 2.6 | 5.4 | 6 |
| AFG1 | 3.8 | 4.1 | 8.1 | 5.9 |
| AFB2 | 4.8 | 8.5 | 7.3 | 9.5 |
| AFB1 | 5.6 | 5.5 | 7.8 | 8.8 |
| HT-2 | 2.9 | 6.8 | 8.7 | 10.2 |
| T-2 | 3.2 | 5.1 | 4.2 | 10.2 |
| OTA | 4.7 | 6.1 | 6.4 | 7.1 |
| ENNB | 2.8 | 5.8 | 3.6 | 7.3 |
| BEA | 4.9 | 5.4 | 7.1 | 7.8 |
| ENNB1 | 2.4 | 3.6 | 4.5 | 5.6 |
| ENNA1 | 2.6 | 4.8 | 4.9 | 8.4 |
| ENNA | 3.5 | 3.6 | 6.8 | 6.9 |
LOD, limit of detection (S/N = 3); LOQ, limit of quantification (S/N = 10); SSE, magnitude of signal suppression/enhancement
Low level: 5 μg kg−1 for AFs, OTA, BEA, and ENNs; 300 μg kg−1 for DON, HT-2, and T-2
High level: 25 μg kg−1 for AFs, OTA, BEA, and ENNs; 500 μg kg−1 for DON, HT-2, and T-2