Table 4.
Sample information São Miguel, Azores archipelago. TTXs analogues in positive samples analyzed by HRMS and quantified by MRM mode.
| Sampling Date | Sampling Site | Sample | Species | Trophic Level [Ref] | Edible | Code | Standard TTX | Suspicious TTXs | RT (min) | Elemental Composition | Theoretical m/z | Experimental m/z | Error (mDa) | TTX eq (µg/Kg) |
|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
| June 2013 | Lagoa | Starfish | Ophidiaster ophidianus | Detritivorous [32] | No | 412 | norTTX | 3.1 | C10H15N3O7 | 290.0983 | 290.2489 | 150.6 | 30,902 | |
| norTTX | 4.6 | C10H15N3O7 | 290.0983 | 290.2303 | 132.0 | 699 | ||||||||
| June 2013 | Ilhéu de São Roque | Starfish | Ophidiaster ophidianus | Detritivorous [32] | No | 424 | norTTX | 3.1 | C10H15N3O7 | 290.0983 | 290.2475 | 149.2 | 42,604 | |
| norTTX | 4.6 | C10H15N3O7 | 290.0983 | 290.2298 | 131.5 | 1638 | ||||||||
| June 2013 | Caloura | Starfish | Ophidiaster ophidianus | Detritivorous [32] | No | 435 | norTTX | 3.1 | C10H15N3O7 | 290.0983 | 290.2478 | 149.9 | 20,853 | |
| June 2013 | Caloura | Fish (Gonads) | Sphoeroides marmoratus | 3rd Level Predator [33] | Yes | 438 G | TTX | 8.1 | C11H17N3O8 | 320.1088 | 320.1088 | 0.0 | 352,886 | |
| 4-epiTTX | 7.8 | C11H17N3O8 | 320.1088 | 320.1082 | −0.6 | 3157 | ||||||||
| deoxyTTX | 7.7 | C11H17N3O7 | 304.1139 | 304.1129 | −1.0 | 446 | ||||||||
| 11-deoxyTTX | 7.0 | C11H17N3O7 | 304.1139 | 304.1126 | −1.3 | 157,156 | ||||||||
| deoxyTTX | 6.5 | C11H17N3O7 | 304.1139 | 304.1124 | −1.5 | 108,375 | ||||||||
| 4,9-anhydroTTX | 7.1 | C11H15N3O7 | 302.0983 | 302.1005 | 2.2 | 91 | ||||||||
| dideoxyTTX | 6.4 | C11H17N3O6 | 288.1190 | 288.1157 | −3.3 | 22,232 | ||||||||
| trideoxyTTX | 5.0 | C11H17N3O5 | 272.1241 | 272.1198 | −4.3 | 12,708 | ||||||||
| trideoxyTTX | 4.8 | C11H17N3O5 | 272.1241 | 272.1228 | −1.3 | 37,367 | ||||||||
| trideoxyTTX | 4.6 | C11H17N3O5 | 272.1241 | 272.1227 | −1.4 | 1849 | ||||||||
| anhydrotrideoxyTTX | 4.7 | C11H15N3O4 | 254.1135 | 254.1122 | −1.3 | 364 | ||||||||
| June 2013 | Caloura | Fish (Liver) | Sphoeroides marmoratus | 3rd Level Predator [33] | Yes | 438 F | TTX | 8.1 | C11H17N3O8 | 320.1088 | 320.1098 | 1.0 | 41 | |
| 4-epiTTX | 7.8 | C11H17N3O8 | 320.1088 | nd | 6 | |||||||||
| 11-deoxyTTX | 7.0 | C11H17N3O7 | 304.1139 | nd | <LOQ | |||||||||
| deoxyTTX | 6.9 | C11H17N3O7 | 304.1139 | nd | 4 | |||||||||
| deoxyTTX | 6.5 | C11H17N3O7 | 304.1139 | 304.1153 | 1.4 | 136 | ||||||||
| 4,9-anhydroTTX | 7.1 | C11H15N3O7 | 302.0983 | nd | <LOQ | |||||||||
| dideoxyTTX | 6.4 | C11H17N3O6 | 288.1190 | nd | 283 | |||||||||
| trideoxyTTX | 5.0 | C11H17N3O5 | 272.1241 | nd | 31 | |||||||||
| trideoxyTTX | 4.8 | C11H17N3O5 | 272.1241 | 272.1263 | 2.2 | 250 | ||||||||
| trideoxyTTX | 4.6 | C11H17N3O5 | 272.1241 | nd | 14 | |||||||||
| June 2013 | Caloura | Fish (Muscle) | Sphoeroides marmoratus | 3rd Level Predator [33] | Yes | 438 M | TTX | 8.1 | C11H17N3O8 | 320.1088 | 320.1088 | 0.0 | 9918 | |
| 4-epiTTX | 7.8 | C11H17N3O8 | 320.1088 | 320.1067 | −2.1 | 118 | ||||||||
| deoxyTTX | 7.7 | C11H17N3O7 | 304.1139 | 304.1164 | 2.5 | 29 | ||||||||
| 11-deoxyTTX | 7.0 | C11H17N3O7 | 304.1139 | 304.1172 | 3.3 | 48 | ||||||||
| deoxyTTX | 6.9 | C11H17N3O7 | 304.1139 | 304.1123 | −1.6 | 65 | ||||||||
| deoxyTTX | 6.5 | C11H17N3O7 | 304.1139 | 304.1100 | −3.9 | 2085 | ||||||||
| 4,9-anhydroTTX | 7.1 | C11H15N3O7 | 302.0983 | 302.0958 | −2.5 | 45 | ||||||||
| dideoxyTTX | 6.4 | C11H17N3O6 | 288.1190 | 288.1145 | −4.5 | 2953 | ||||||||
| trideoxyTTX | 5.0 | C11H17N3O5 | 272.1241 | nd | 122 | |||||||||
| trideoxyTTX | 4.8 | C11H17N3O5 | 272.1241 | 272.1217 | −2.4 | 507 | ||||||||
| trideoxyTTX | 4.6 | C11H17N3O5 | 272.1241 | nd | 26 | |||||||||
| anhydrotrideoxyTTX | 4.7 | C11H15N3O4 | 254.1135 | 254.1129 | −0.6 | 5 |
nd—not detected.