Table 7.
Validation results of the in-house cross-validation of the UPLC MS/MS method with rumen fluid–buffer mixture and maize silage (10 mg/mL) for within-run precision (n = 6) with corresponding accuracy at low (LOQ), medium, and high concentration level. The different concentration levels for each mycotoxin are mentioned in Table 6. For all components, the acceptability ranges for accuracy and precision were met.
| Analyte | Within-Run (n = 6) | |||||
|---|---|---|---|---|---|---|
| Accuracy (%) | Precision (RSD, %) | |||||
| LOQ | Medium | High | LOQ | Medium | High | |
| DON | −0.3 B | 0.1 C | −4.8 C | 0.6 B | 2.5 C | 3.6 D |
| DOM-1 | −7.9 B | −6.3 C | 1.9 C | 9.7 B | 3.3 C | 4.7 D |
| NIV | 1.1 C | 5.5 C | −1.0 C | 5.6 C | 2.8 D | 8.0 D |
| ENN B | −2.0 A | 4.5 B | −8.5 C | 4.0 A | 2.9 B | 5.1 C |
| MPA | −1.1 B | −7.3 B | 3.6 C | 5.0 B | 8.9 B | 7.4 C |
| ROQ-C | −12.5 A | −1.0 B | −5.2 C | 3.1 A | 3.3 B | 3.0 C |
| ZEN | −6.0 B | 2.5 B | 3.1 C | 8.8 B | 6.2 B | 7.3 C |
| ZAN | −2.2 A | 0.9 B | 8.3 C | 6.0 A | 4.7 B | 0.9 C |
| α-ZEL | 1.9 A | −7.6 B | −5.2 C | 4.7 A | 2.9 B | 6.5 C |
| β-ZEL | −1.4 A | −17.6 B | −0.7 C | 8.2 A | 10.0 B | 7.8 C |
| α-ZAL | −10.9 B | −17.0 B | 7.4 C | 7.8 B | 9.5 B | 6.7 C |
| β-ZAL | −8.3 A | −16.8 B | −2.9 C | 6.4 A | 11.1 B | 7.5 C |
Note: DON = deoxynivalenol, DOM-1 = deepoxy-deoxynivalenol, NIV = nivalenol, ENN B = enniatin B, MPA = mycophenolic acid, ROQ-C = roquefortine C, ZEN = zearalenone, ZAN = zearalanone, α-ZEL = α-zearalenol, β-ZEL = β-zearalenol, α-ZAL = α-zearalanol, and β-ZAL = β-zearalanol. Acceptability ranges for accuracy: −50 to +20% for conc. <1 ng/mL (A in superscript), −30 to +10% for conc. ≥1 to 10 ng/mL (B in superscript), −20% to +10% for conc. ≥10 ng/mL (C in superscript), and within-run precision: RSDmax = 30% for conc. <1 ng/mL (A in superscript), RSDmax = 25% for conc. ≥1 to 10 ng/mL (B in superscript), RSDmax = 15% for conc. ≥10 ng/mL to 100 ng/mL (C in superscript), RSDmax = 10% for conc. ≥100 ng/mL (D in superscript).