Table 2.
Method validation parameters including spiking levels, limits of detection (LOD) and quantitation (LOQ), linear range, extraction efficiency (RE), intermediate precision (RSDR) and repeatability (RSDr), as well as signal suppression and enhancement (SSE)
| Analytes | Spiking levelsa | LODb, c | LOQd, c | Rangee | REf ± RSDRg | RSDrh | SSEi | ||||||
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| [ng/g] | [ng/g] | [ng/g] | [ng/mL] | [%] | [%] | [%] | |||||||
| T | O | F | T | O | F | T | O | F | |||||
| AOH | 5/25/125 | 0.5/0.1/0.6 | 1.0/0.2/1.2 | 0.05–100 | 87 ± 11 | 95 ± 15 | 94 ± 11 | 15/4/3 | 35/11/3 | 29/10/4 | 94 | 102 | 95 |
| AME | 1/5/25 | 0.05/0.03/0.05 | 0.1/0.06/0.1 | 0.01–20 | 86 ± 10 | 84 ± 25 | 99 ± 11 | 9/3/5 | 20/6/5 | 11/6/3 | 81 | 93 | 124 |
| ALT | 30/150/750 | 5.0/5.5/6.0 | 10/11/12 | 0.3–600 | 77 ± 15 | 91 ± 13 | 94 ± 13 | 22/15/4 | 22/15/8 | 14/8/8 | 99 | 109 | 112 |
| isoALT | 30/150/750 | 3.5/3.0/4.0 | 7/8/9 | 0.3–600 | 78 ± 24 | 83 ± 17 | 96 ± 16 | 23/32/4 | 30/8/3 | 21/8/6 | 101 | 105 | 99 |
| TeA | 60/300/1500 | 6/4/7 | 12/8/14 | 0.6–1200 | 77 ± 13 | 75 ± 12 | 91 ± 15 | 22/11/6 | 16/8/5 | 19/10/6 | 90 | 98 | 83 |
| TEN | 1.5/7.5/37.5 | 0.1/0.05/0.5 | 0.2/0.1/1.0 | 0.015–30 | 84 ± 19 | 98 ± 25 | 92 ± 21 | 34/18/8 | 33/8/6 | 19/21/7 | 90 | 111 | 83 |
| AOH-3-Glc | 5/25/125 | 1.0/0.8/1.0 | 2.0/1.6/2.0 | 0.05–100 | 81 ± 20 | 94 ± 16 | 94 ± 16 | 28/14/5 | 32/9/3 | 23/8/3 | 51 | 118 | 68 |
| AOH-9-Glc | 20/100/500 | 4.5/8.0/6.0 | 9/16/12 | 1.2–400 | 85 ± 44 | 83 ± 29 | 86 ± 27 | 19/38/17 | 7/28/16 | 42/39/12 | 79 | 114 | 72 |
| AOH-3-S | 5/25/125 | 1.0/1.8/1.0 | 2.0/3.6/2.0 | 0.05–100 | 82 ± 12 | 91 ± 15 | 55 ± 20 | 19/9/3 | 28/10/5 | 31/15/7 | 84 | 101 | 97 |
| AME-3-Glc | 10/50/250 | 2.0/2.0/1.0 | 4.0/4.0/2.0 | 0.2–200 | 82 ± 34 | 93 ± 25 | 87 ± 38 | 19/23/12 | 40/12/11 | 53/30/5 | 97 | 104 | 103 |
| AME-3-S | 5/25/125 | 0.05/0.05/0.1 | 0.1/0.1/0.2 | 0.05–100 | 84 ± 12 | 100 ± 9 | 59 ± 12 | 9/5/4 | 8/6/3 | 16/4/3 | 107 | 95 | 156 |
| ATX-I | 1/5/25 | 0.2/0.5/0.6 | 0.4/1.0/1.2 | 0.02–20 | 79 ± 22 | 92 ± 20 | 84 ± 29 | 16/21/16 | 48/20/8 | 83/15/11 | 103 | 102 | 89 |
| ATX-II | 5/25/125 | 0.5/1.5/1.2 | 1.0/3.0/2.4 | 0.05–100 | 81 ± 14 | 80 ± 19 | 83 ± 23 | 34/10/10 | 32/8/8 | 29/28/8 | 101 | 102 | 96 |
| ALP | 5/25/125 | 0.8/1.0/1.0 | 1.6/2.0/2.0 | 0.05–100 | 75 ± 21 | 89 ± 24 | 79 ± 28 | 33/13/12 | 28/18/6 | 45/22/4 | 103 | 103 | 97 |
| STTX-III | 5/25/0 | 0.5/3.0/1.0 | 1.0/6.0/2.0 | 0.3–10 | 51 ± 49 | 94 ± 32 | 28 ± 71 | 31/29/– | 22/19/– | 75/19/– | 106 | 113 | 144 |
| ALS | 30/150/750 | 1.8/8.0/9.0 | 3.6/16.0/18.0 | 0.3–600 | 77 ± 9 | 97 ± 20 | 19 ± 29 | 11/5/2 | 23/18/7 | –/13/22 | 144 | 14 | 56 |
| AA-III | 10/50/250 | 1.5/1.5/1.8 | 3.0/3.0/3.6 | 0.1–200 | 83 ± 14 | 88 ± 11 | 64 ± 26 | 10/9/7 | 15/10/4 | 23/16/12 | 104 | 106 | 131 |
aFortification levels were identical for the three matrices (tomato sauce, T; sunflower seed oil, O; wheat flour, F) chosen for low/middle/high concentrations
bLimit of detection
cValues in the following order: tomato sauce/sunflower seed oil/wheat flour matrix
dLimit of quantitation
eConcentration range with linear regression
fRelative recovery (extraction efficiency), calculated as the ratio of analyte concentration quantified using the matrix-matched calibration curve and the known spiking level in the fortified blank samples, averaged over the results of the three spiking levels
gIntermediate precision (interday precision), calculated from the standard deviations of the samples spiked at three levels and measured on three different days of the three consecutive weeks, averaged over the results of the three spiking levels
hRepeatability (intraday precision), calculated from the standard deviations of the samples spiked at three levels measured twice within the same sequence
iSignal suppression and enhancement, calculated as the ratio of calibration curve slopes of the respective matrix and neat solvent