Table 2.
UPLC-MS/MS Conditions for the Detection of Cyclic Imine Toxin Standards in Methanol and in Shellfish Matrixesa
| 13,19-didesmethyl spirolide-C |
13-desmethyl spirolide-C |
pinnatoxin-G | 20-methyl spirolide-G |
gymnodimine- A | pinnatoxin-A | |
|---|---|---|---|---|---|---|
| MRM transition (m/z) | 678.4 > 164.1 | 692.4 > 444.4 | 694.38 > 676.36 | 706.50 > 688.38 | 508.4 > 490.4 | 712.4 > 164.0 |
| cone voltage (V) | 50 | 60 | 75 | 65 | 50 | 65 |
| collision energy (eV) | 40 | 35 | 30 | 30 | 32 | 48 |
| retention time (min) | 6.12 | 7.20 | 8.42 | 7.89 | 4.71 | 6.17 |
| LOD per column (methanol) | 10 pM or 0.014 pg | 100 pM or 0.14 pg | 100 pM or 0.14 pg | 100 pM or 0.14 pg | 100 pM or 0.10 pg | 100 pM or 0.14 pg |
| LOQ per column (methanol) | 1 nM or 1.35 pg | 1 nM or 1.38 pg | 1 nM or 1.39 pg | 1 nM or 1.41 pg | 1 nM or 1.0 pg | 1 nM or 1.42 pg |
| R2 (methanol) | 0.9999 | 0.9999 | 0.9998 | 1.0000 | 0.9999 | 1.0000 |
| R2 (mussels) | 0.9632 | 0.9588 | 0.9565 | 0.9616 | 0.9605 | 0.9583 |
| LOD per column (bibliography) | – | 0.8 pg,37 0.2 pg36 | – | – | 3.7 pg,37 0.6 pg36 | – |
a
Abbreviations: MRM, multiple-reaction-monitoring mode; LOD, limit of detection (obtained from low-level standards with a signal-to-noise ratio equal to 3); LOQ, limit of quantification (obtained from low-level standards with a signal-to-noise ratio equal to 10).