Table 2.
Sampling data | Prorocentrum minimum (cells/L) | MBA (Yasumoto1978 [39]) | MBA (Other) | UPLC-MS/MS | |||||||||||
---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|---|
Sample code | Date of collection | Regional Unit | Site | Species | Result | Symptomatology | Protocol | Result | Symptomatology | Tissue tested | TTX (μg/kg) | 4-epi-TTX (μg/kg) | 4,9-anhydro-TTX (μg/kg) | Sum of TTXs (μg/kg) | |
1727/2012 | 7 May 2012 | Rodopi | Zone 6 | Mussels | Presence | Negative (− − −) | No symptomatology | N/A | N/A | N/A | DG | 46.2 | ND | ND | 46.2 |
1770/2012 | 22 May 2012 | Rodopi | Zone 6 | Mussels | 8.26× 102 | Positive (+ + +) | 3/3 mice dead in 1:00–1:30 h | CRL-MBA-SOP v.5 (DEE fraction) | Negative (− − −) | None | DG | 202.9 | 7.6 | <LOQ (12.4) * | 222.9 |
WF | 179.1 | <LOQ (4.2) * | <LOQ (10.3) * | 193.6 | |||||||||||
1774/2012 | 28 May 2012 | Rodopi | Zone 6 | Mussels | 1.78 × 103 | Positive (+ + +) | 3/3 mice dead in 1:30–2:00 h | CRL-MBA-SOP v.5 (DEE fraction) | Negative (− − −) | 2/3 mice with mild diarrhea | DG | 185.9 | <LOQ (4.5) * | <LOQ (15.9) * | 206.3 |
1786/2012 | 30 May 2012 | Rodopi | Zone 6 | Mussels | 1.70 × 103 | Positive (+ + +) | 3/3 mice dead (1/3 in 1:15–1:30 h, 1/3 in 1:48 h & 1/3 in 1:51 h) | CRL-MBA-SOP v.5 (DEE fraction) | Negative (− − −) | 1/3 mice with mild diarrhea | DG | 180.0 | <LOQ (6.8) * | <LOQ (14.5) * | 201.4 |
CRL-MBA-SOP v.5 (aqueous fraction) | Positive (+ + +) | 3/3 mice dead in 7–10 min | |||||||||||||
1798/2012 | 6 Jun 2012 | Rodopi | Zone 6 | Mussels | 1.89 × 103 | Positive (+ + +) | 3/3 mice dead (1/3 in 1:31 h, 1/3 in 2:30 h & 1/3 in 2:31) | CRL-MBA-SOP v.5 (DEE fraction) | Negative (− − −) | None | DG | 186.2 | 15.6 | <LOQ (14.7) * | 216.6 |
1801/2012 | 11 Jun 2012 | Rodopi | Zone 6 | Mussels | 5.65 × 102 | Negative (− − −) | 2/3 mice with diarrhoea | CRL-MBA-SOP v.5 (ether fraction) | Negative (− − −) | 1/3 mice with diarrhea | DG | 56.5 | 8.8 | 22.9 | 88.2 |
MBA = Mouse bioassay, TTX = tetrodotoxin, DG = digestive glands, WF = whole flesh, DEE = diethylether, N/A = not applicable, ND = not detected. Values with an asterisk (*) indicate concentrations between the calculated method LOD and LOQ and are shown as contributions to the sum of TTXs.