Table 3.
Performance validation parameters for the multi-analyte LC-HRMS/MS method (n = number of analysis for each category; a: solvent; b: fish feed; c: salmon; d: zebrafish).
| Compound | n | LOD | LOQ | SSE (%) |
Total within Laboratory Precision (%) |
Recovery ± SD (%) |
||||||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| (µg/L) | (µg/kg) | (µg/L) | (µg/kg) | |||||||||||||
| (a/b/c/d) | (a) | (b) | (c) | (d) | (a) | (b) | (c) | (d) | (b/c/d) | (b) | (c) | (b) | (c) | (d) | ||
| with ISTD | ||||||||||||||||
| DON | 4/4/3/3 | 3 | 23 | 67 | 22 | 9 | 78 | 225 | 74 | 77/87/133 | 4 | 4 | 90 ± 7 | 107 ± 13 | 92 ± 25 | |
| 3-ADON | 4/4/3/3 | 4 | 17 | 57 | 9 | 15 | 56 | 189 | 29 | 98/116/144 | 3 | 3 | 112 ± 17 | 96 ± 12 | 78 ± 20 | |
| 15-ADON | 4/3/3/3 | 5 | 6 | 43 | 63 | 16 | 20 | 142 | 210 | 96/161/141 | 10 | 3 | 133 ± 2 | 107 ± 25 | 86 ± 14 | |
| DON-3G | 4/4/3/3 | 5 | 36 | 115 | 176 | 18 | 121 | 383 | 588 | 85/95/119 | 11 | 22 | 19 ± 9 | 83 ± 20 | 48 ± 31 | |
| NIV | 4/4/3/3 | 19 | 59 | 144 | 76 | 63 | 196 | 479 | 252 | 71/65/115 | 17 | 41 | 57 ± 34 | 69 ± 33 | 41 ± 24 | |
| T-2 | 4/4/3/3 | 4 | 26 | 53 | 26 | 12 | 88 | 176 | 86 | 97/136/151 | 3 | 3 | 96 ± 17 | 99 ± 15 | 90 ± 19 | |
| HT-2 | 4/4/3/3 | 2 | 22 | 70 | 15 | 8 | 73 | 235 | 52 | 89/129/149 | 2 | 3 | 94 ± 18 | 96 ± 11 | 98 ± 15 | |
| OTA | 4/4/3/3 | 5 | 41 | 44 | 21 | 18 | 138 | 148 | 68 | 105/139/150 | 6 | 4 | 75 ± 13 | 87 ± 23 | 83 ± 20 | |
| ZEN | 4/4/3/3 | 6 | 11 | 43 | 14 | 22 | 38 | 143 | 47 | 90/125/125 | 1 | 2 | 109 ± 5 | 106 ± 18 | 96 ± 25 | |
| Ergonovine | 4/4/3/3 | 6 | 23 | 35 | 8 | 19 | 77 | 115 | 26 | 85/130/106 | 2 | 1 | 84 ± 8 | 98 ± 13 | 87 ± 30 | |
| Ergosine | 4/4/3/3 | 4 | 35 | 52 | 9 | 12 | 117 | 173 | 32 | 79/129/138 | 7 | 11 | 69 ± 27 | 89 ± 31 | 72 ± 20 | |
| Ergotamine | 4/4/3/3 | 2 | 59 | 56 | 10 | 8 | 195 | 188 | 35 | 81/134/155 | 10 | 9 | 64 ± 10 | 84 ± 26 | 77 ± 18 | |
| Ergocornine | 4/4/3/3 | 3 | 32 | 59 | 16 | 11 | 108 | 196 | 53 | 93/129/136 | 11 | 11 | 59 ± 16 | 90 ± 26 | 70 ± 14 | |
| α-Ergocryptine | 4/4/3/3 | 4 | 15 | 38 | 8 | 14 | 50 | 126 | 28 | 67/119/137 | 7 | 8 | 53 ± 7 | 82 ± 21 | 70 ± 14 | |
| Ergoscristine | 4/4/3/3 | 3 | 30 | 51 | 10 | 10 | 100 | 170 | 32 | 70/117/135 | 8 | 5 | 77 ± 22 | 88 ± 24 | 54 ± 26 | |
| without ISTD | ||||||||||||||||
| ENN A | 4/4/3/3 | 4 | 85 | 49 | 32 | 13 | 284 | 165 | 108 | 115/173/181 | 1 | 8 | 161 ± 14 | 117 ± 27 | 81 ± 17 | |
| ENN A1 | 4/4/3/3 | 1 | 45 | 40 | 33 | 5 | 150 | 133 | 111 | 102/122/148 | 3 | 11 | 147 ± 21 | 110 ± 29 | 80 ± 16 | |
| ENN B | 4/4/3/3 | 1 | 41 | 78 | 17 | 4 | 138 | 260 | 57 | 95/132/152 | 2 | 10 | 117 ± 16 | 107 ± 30 | 79 ± 17 | |
| ENN B1 | 4/4/3/3 | 1 | 29 | 40 | 29 | 5 | 96 | 133 | 96 | 102/125/147 | 3 | 12 | 134 ± 9 | 106 ± 35 | 79 ± 17 | |
| Daidzein | 4/4/3/3 | 13 | 30 | 50 | 48 | 42 | 100 | 168 | 159 | 86/120/101 | 4 | 13 | 123 ± 9 | 122 ± 18 | 93 ± 15 | |
| Daidzin | 4/4/3/3 | 3 | 19 | 45 | 15 | 12 | 62 | 152 | 51 | 86/113/140 | 4 | 16 | 93 ± 21 | 93 ± 6 | 71 ± 13 | |
| Genistein | 4/4/3/3 | 11 | 20 | 42 | 52 | 37 | 66 | 141 | 172 | 81/120/104 | 2 | 13 | 114 ± 23 | 127 ± 28 | 91 ± 18 | |
| Genistin | 4/4/3/3 | 1 | 29 | 72 | 11 | 5 | 95 | 241 | 35 | 101/143/149 | 4 | 12 | 101 ± 45 | 88 ± 1 | 69 ± 14 | |
| Glycitein | 4/4/3/3 | 11 | 18 | 21 | 37 | 36 | 58 | 68 | 124 | 80/58/89 | 2 | 16 | 127 ± 3 | 118 ± 24 | 96 ± 16 | |
| Glycitin | 4/4/3/3 | 4 | 27 | 51 | 26 | 13 | 90 | 170 | 88 | 94/123/121 | 4 | 23 | 96 ± 14 | 113 ± 13 | 97 ± 22 | |