Table 2.
GC -NICI -MS method validation data after sulfate cleavage (method B)
| 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 | 0.49 | −1.8 | 3.1 | 5.5 | 121 (8/3) | 0.1–25 | Quadratic 1/X | R-MDA d5 | 0.005 | 0.1 |
| MED | 7.5 | 7.1 | −4.7 | 1.2 | 2.6 | – | ||||||
| HIGH | 20.0 | 19.4 | −3.1 | 5.9 | 8.1 | 101 (3/2) | ||||||
| S-MDA | LOW | 0.50 | 0.47 | −5.4 | 7.0 | 8.2 | 128 (6/2) | 0.1–25 | Quadratic 1/X | S-MDA d5 | 0.005 | 0.1 |
| MED | 7.5 | 7.2 | −4.3 | 3.5 | 4.2 | – | ||||||
| HIGH | 20.0 | 19.1 | −4.6 | 5.6 | 8.9 | 101 (3/0.3) | ||||||
| R-HMA | LOW | 0.50 | 0.50 | −0.4 | 11.0 | 15.5 | 109(10/5) | 0.1–25 | Quadratic log log | S-Pholedrine | 0.025 | 0.1 |
| MED | 7.5 | 7.7 | 2.4 | 7.0 | 9.5 | – | ||||||
| HIGH | 20.0 | 20.5 | 2.6 | 13.3 | 14.2 | 97(3/5) | ||||||
| S-HMA | LOW | 0.50 | 0.51 | 1.5 | 10.0 | 19.3 | 106(10/5) | 0.1–25 | Quadratic log log | S-Pholedrine | 0.025 | 0.1 |
| MED | 7.5 | 7.6 | 1.7 | 5.1 | 8.7 | – | ||||||
| HIGH | 20.0 | 20.5 | 2.4 | 13.2 | 13.6 | 96 (2/6) | ||||||
| R-DHA | LOW | 0.50 | 0.45 | −11.0 | 9.2 | 13.6 | 48 (46/19) | 0.25–25 | Quadratic log log | DHBA | 0.25 | 0.25 |
| MED | 7.5 | 7.1 | −4.7 | 7.4 | 10.9 | – | ||||||
| HIGH | 20.0 | 18.9 | −5.5 | 8.6 | 8.8 | 51 (38/13) | ||||||
| S-DHA | LOW | 0.50 | 0.42 | −15.3 | 7.4 | 13.0 | 48 (53/15) | 0.25–25 | Quadratic log log | DHBA | 0.25 | 0.25 |
| MED | 7.5 | 7.3 | −2.9 | 6.0 | 9.4 | – | ||||||
| HIGH | 20.0 | 19.2 | −3.8 | 8.7 | 10.2 | 56 (34/12) | ||||||
| R-MDMA | LOW | 0.50 | 0.39 | −22.5 | 7.5 | 11.1 | 123 (6/6) | 0.1–125 | Quadratic log log | R-MDMA d5 | 0.005 | 0.1 |
| MED | 35.0 | 35.4 | 1.1 | 1.8 | 5.1 | – | ||||||
| HIGH | 100.0 | 99.1 | −0.9 | 5.0 | 6.4 | 97(2/2) | ||||||
| S-MDMA | LOW | 0.50 | 0.41 | −18.6 | 6.5 | 11.3 | 118 (5/3) | 0.1–125 | Quadratic log log | S-MDMA d5 | 0.005 | 0.1 |
| MED | 35.0 | 35.3 | 0.8 | 2.0 | 4.8 | – | ||||||
| HIGH | 100.0 | 99.7 | −0.3 | 4.5 | 6.2 | 97 (3/3) | ||||||
| R-HMMA | LOW | 0.50 | 0.45 | −9.1 | 10.5 | 18.3 | 97 (17/11) | 0.1–125 | Quadratic log log | S-Pholedrine | 0.05 | 0.1 |
| MED | 35.0 | 38.9 | 11.2 | 6.0 | 8.7 | – | ||||||
| HIGH | 100.0 | 102.7 | 2.7 | 8.8 | 9.3 | 95 (4/3) | ||||||
| S-HMMA | LOW | 0.50 | 0.45 | −10.1 | 8.9 | 15.5 | 95(10/7) | 0.1–125 | Quadratic log log | S-Pholedrine | 0.05 | 0.1 |
| MED | 35.0 | 39.0 | 11.3 | 5.5 | 8.3 | – | ||||||
| HIGH | 100.0 | 101.9 | 1.9 | 7.8 | 8.9 | 94 (4/3) | ||||||
| R-DHMA | LOW | 0.50 | 0.43 | −13.8 | 11.6 | 17.7 | 17 (54/12) | 0.25–37.5 | Quadratic 1/X | DHBA | 0.25 | 0.25 |
| MED | 10.0 | 10.4 | 4.1 | 14.0 | 14.5 | – | ||||||
| HIGH | 35.0 | 33.6 | −4.0 | 8.7 | 12.1 | 19 (59/14) | ||||||
| S-DHMA | LOW | 0.50 | 0.42 | −16.5 | 14.5 | 19.2 | 16 (74/10) | 0.25–37.5 | Quadratic 1/X | DHBA | 0.25 | 0.25 |
| MED | 10.0 | 10.5 | 5.3 | 12.0 | 14.5 | – | ||||||
| HIGH | 35.0 | 33.6 | −4.0 | 8.1 | 10.3 | 19 (60/14) | ||||||
| R-HMMA sulfate | MED | 12.5 | 13.6 | 8.8 | 8.3 | 11.4 | – | – | – | – | – | – |
| S-HMMA sulfate | MED | 12.5 | 13.8 | 10.1 | 10.0 | 11.8 | – | – | – | – | – | – |
| R-DHMA sulfate | MED | 20.0 | 16.7 | −16.4 | 10.2 | 12.7 | – | – | – | – | – | – |
| S-DHMA sulfate | MED | 20.0 | 16.0 | −20.0 | 11.0 | 14.3 | – | – | – | – | – | – |
Bold values indicate values outside the acceptance criteria of ±15% or ±20%