Table 3.
GC-NICI-MS method validation data (method C)
| Analyte | QC sample | Nominal concentration (µM) |
Mean calculated concentration (µM) |
Accuracy (%) |
Intra-day precision (%) |
Inter-day precision (%) |
RE (%), (CV%/CV% IS corrected) |
Calibration range (µM) |
Calibration model | Internal standard | LOD (µM) |
LOQ (µM) |
|---|---|---|---|---|---|---|---|---|---|---|---|---|
| R-MDA | LOW | 0.50 | 0.50 | −0.3 | 4.3 | 9.5 | 108(13/1) | 0.1–25 | Quadratic MX | R-MDA d5 | 0.005 | 0.1 |
| MED | 7.5 | 7.2 | −4.4 | 2.3 | 4.3 | – | ||||||
| HIGH | 20.0 | 18.6 | −7.2 | 2.7 | 9.4 | 109(6/1) | ||||||
| S-MDA | LOW | 0.50 | 0.48 | −3.7 | 4.9 | 8.6 | 116(12/4) | 0.1–25 | Quadratic MX | S-MDA d5 | 0.005 | 0.1 |
| MED | 7.5 | 7.3 | −3.2 | 3.4 | 3.1 | – | ||||||
| HIGH | 20.0 | 18.9 | −5.5 | 2.8 | 8.7 | 106(5/2) | ||||||
| R-HMA | LOW | 0.50 | 0.46 | −8.6 | 8.9 | 12.9 | 98(17/5) | 0.1–25 | Quadratic log log | S-Pholedrine | 0.025 | 0.1 |
| MED | 7.5 | 7.6 | 1.5 | 9.4 | 8.0 | – | ||||||
| HIGH | 20.0 | 20.0 | −0.1 | 6.6 | 11.4 | 97 (8/4) | ||||||
| S-HMA | LOW | 0.50 | 0.46 | −8.5 | 7.1 | 11.4 | 93(17/5) | 0.1–25 | Quadratic og log | S-Pholedrine | 0.025 | 0.1 |
| MED | 7.5 | 7.5 | −0.4 | 8.9 | 7.8 | – | ||||||
| HIGH | 20.0 | 20.0 | −0.1 | 7.2 | 10.9 | 99 (7/4) | ||||||
| R-DHA | LOW | 0.50 | 0.44 | −11.0 | 4.9 | 9.9 | 43 (47/7) | 0.25–25 | Quadratic log log | DHBA | 0.05 | 0.25 |
| MED | 7.5 | 7.2 | −3.3 | 4.8 | 7.7 | – | ||||||
| HIGH | 20.0 | 18.2 | −8.9 | 5.8 | 8.2 | 53 (55/5) | ||||||
| S-DHA | LOW | 0.50 | 0.43 | −14.4 | 6.4 | 10.2 | 49 (45/8) | 0.25–25 | Quadratic log log | DHBA | 0.05 | 0.25 |
| MED | 7.5 | 7.3 | −2.7 | 10.6 | 11.5 | – | ||||||
| HIGH | 20.0 | 18.0 | −10.2 | 6.2 | 11.3 | 54 (52/6) | ||||||
| R-MDMA | LOW | 0.50 | 0.41 | −18.7 | 8.7 | 15.0 | 107(15/8) | 0.1–125 | Quadratic log log | R-MDMA d5 | 0.005 | 0.1 |
| MED | 35.0 | 36.2 | 3.3 | 1.8 | 5.8 | – | ||||||
| HIGH | 100.0 | 95.6 | −4.4 | 2.2 | 8.7 | 105(5/4) | ||||||
| S-MDMA | LOW | 0.50 | 0.42 | −16.2 | 8.9 | 15.6 | 104(15/5) | 0.1–125 | Quadratic log log | S-MDMA d5 | 0.005 | 0.1 |
| MED | 35.0 | 36.2 | 3.3 | 1.8 | 5.6 | – | ||||||
| HIGH | 100.0 | 96.6 | −3.4 | 2.5 | 7.9 | 106(5/4) | ||||||
| R-HMMA | LOW | 0.50 | 0.43 | −14.0 | 9.5 | 15.4 | 83 (20/8) | 0.1–125 | Quadratic log log | S-Pholedrine | 0.05 | 0.1 |
| MED | 35.0 | 37.8 | 8.1 | 6.7 | 5.8 | – | ||||||
| HIGH | 100.0 | 99.1 | −0.9 | 5.8 | 10.9 | 99 (8/2) | ||||||
| S-HMMA | LOW | 0.50 | 0.41 | −17.1 | 9.8 | 13.1 | 81 (18/7) | 0.1–125 | Quadratic log log | S-Pholedrine | 0.05 | 0.1 |
| MED | 35.0 | 38.1 | 8.7 | 6.5 | 5.9 | – | ||||||
| HIGH | 100.0 | 97.8 | −2.2 | 4.8 | 10.3 | 99 (9/2) | ||||||
| R-DHMA | LOW | 0.50 | 0.43 | −14.1 | 7.1 | 9.1 | 20 (56/9) | 0.25–37.5 | Quadratic 1/X | DHBA | 0.05 | 0.25 |
| MED | 10.0 | 10.6 | 6.1 | 5.5 | 9.1 | – | ||||||
| HIGH | 35.0 | 33.8 | −3.5 | 3.9 | 7.8 | 26 (80/10) | ||||||
| S-DHMA | LOW | 0.50 | 0.42 | −15.7 | 8.9 | 12.6 | 19 (62/15) | 0.25–37.5 | Quadratic 1/X | DHBA | 0.05 | 0.25 |
| MED | 10.0 | 10.7 | 7.2 | 5.8 | 8.1 | – | ||||||
| HIGH | 35.0 | 33.7 | −3.7 | 3.8 | 7.4 | 28 (76/10) |
Bold values indicate values outside the acceptance criteria of ±15% or ±20%