Fig. 1
Fig. 2
Various LC–MS studies on the determination of TTX and its analogues
| Mobile phase | Column | Linear range | LOD and LOQ | Recovery | Matrix | Reference |
|---|---|---|---|---|---|---|
| 1% acetonitrile, 20 mM ammonium 10 mM ammonium heptafluorobutyrate, formate (pH 4.0) | Reversed (250 × 4.6 phase mm) | 0.05–1 nM | LOD LOQ – – 0.7 NR pM | NR | Puffer fish | (56) |
| 20 mM ammonium acetate, methanol (75/25, v/v) | Reversed phase (150 × 4.6 mm) | 0.01–1 μg/mL | LOD – 0.1 μg/g LOQ – NR | 77.7– 80.7% | Puffer fish | (17) |
| 30 mM heptafluorobutyric acid, 1 mM ammonium acetate (pH 5) | Reversed phase (250 × 4.6 mm) | NR | NR | NR | Japanese fire belly newt (Cynops pyrrhogaster) | (41) |
| A: 0.1% formic acid in water B: methanol | HILIC (150 × 4.6 mm) | 1–100 ng/mL | LOD – 0.1 ng/mL LOQ – 1 ng/mL | > 95% | Human blood serum | (30) |
| 16 mM ammonium formate buffer (pH 5.5), acetonitrile (3/7, v/v) | HILIC (5 μm, 150 × 2 mm) | NR | LOD – 0.5 nM/g LOQ – NR | NR | Puffer fish | (27) |
| 10 mM/L ammonium formate, formic acid (95/5, v/v), 5 mM heptafluorobutyric acid, 2% acetonitrile | Reversed phase (5 μm, 2.1 × 15 mm) | 0–500 ng/mL in urine samples 0–20 ng/mL for plasma samples | LOD – 0.13 ng/mL LOQ – 2.5 ng/mL | 75–81% | Human urine and plasma | (12) |
| A: 10 mM ammonium formate, 10 mM formic acid in water B: acetonitrile, water (95/5, v/v), 5 mM ammonium formate, 2 mM formic acid | HILIC (3.5 μm, 150 × 2.1 mm) | 62.5–2,000 ng/mL | LOD – 16 ng/mL LOQ – 63 ng/mL | NR | Puffer fish | (54) |
| A: 5% acetonitrile B: 95% acetonitrile, 1% acetic acid (pH 3.5) | HILIC (1.7 μm, 100 × 2.1 mm) | 5–500 ng/mL | LOD – 0.074 ng/mL LOQ – 0.123 ng/mL | 80–92% | Gastropod | (48) |
Cases of TTX poisoning
| Country | Source of TTX | Number of cases | Reference |
|---|---|---|---|
| Japan | Puffer fish | 1 | (49) |
| Japan | Puffer fish | 11 | (13) |
| Thailand | Eggs of horseshoe crab (Carcinoscorpius rotundicauda) | 71 | (31) |
| Japan | Puffer fish | 1 | (64) |
| Bangladesh | Puffer fish | 8 | (37) |
| China | Gastropods | 30 | (59) |
| Australia | Puffer fish | 11 | (25) |
| Taiwan | Gastropods | 4 | (21) |
| Taiwan | Puffer fish | 6 | (18) |
| Taiwan | Gastropods | 1 | (23) |
| Australia | Toadfish | 7 | (50) |
| Taiwan | Gastropods | 6 | (22) |
| Bangladesh | Puffer fish | 36 | (1) |
| Japan | Puffer fish | 7 | (2) |
| Taiwan | Puffer fish | 5 | (20) |
| Taiwan | Gastropods | 1 | (29) |
| Taiwan | Gastropods | 3 | (30) |
| Spain | Trumpet shell(Charonia lampas) | 1 | (55) |
| Japan | Puffer fish, Thread-sail filefish, Marine snail | 3 | (3) |
| Spain | Trumpet shell(Charonia sauliae) | 1 | (11) |
| Taiwan | Gastropods | 5 | (47) |
| South Korea | Puffer fish | 3 | (6) |
| China | Goby fish | 22 | (68) |