Table 2.
Confirmation with LTQ Orbitrap Discovery® FT-MS and quantification with 3200QTrap® of SPX-1 and PnTX-G in shellfish. ND: Not detected; NC: Not confirmed; NQ: Not quantified. Δ ppm: mass error in ppm; [M + H]+: Molecular Ion (SPX-1: 692.4521 m/z; PnTX-G: 694.4677 m/z); Fragment 1: 164.1434 m/z (both SPX-1 and PnTX-G); Fragment 2: 444.3108 (SPX-1) and 458.3265 m/z (PnX-G); Fragment 3: 674.4415 m/z (SPX-1) and 676.4572 m/z (PnTX-G).
| Sample Details | SPX-1 (Δ ppm) | SPX-1 (μg/kg) | PnTX-G (Δ ppm) | PnTX-G (μg/kg) | ||
|---|---|---|---|---|---|---|
| OYS110102 | [M + H]+ | 1.0 | [M + H]+ | Δppm > 5 ppm | ||
| Oyster | Frag 1 | −0.2 | 3.6 ± 0.1 | Frag 1 | Δppm > 5 ppm | ND |
| January 2011 | Frag 2 | 1.2 | Frag 2 | Δppm > 5 ppm | ||
| Fangar Bay | Frag 3 | −2.3 | Frag 3 | Δppm > 5 ppm | ||
| OYS110103 | [M + H]+ | −0.2 | [M + H]+ | Δppm > 5 ppm | ||
| Oyster | Frag 1 | 0.2 | 3.5 ± 0.8 | Frag 1 | Δppm > 5 ppm | ND |
| January 2011 | Frag 2 | −0.9 | Frag 2 | Δppm > 5 ppm | ||
| Fangar Bay | Frag 3 | −3.5 | Frag 3 | Δppm > 5 ppm | ||
| OYS110105 | [M + H]+ | 5.0 | [M + H]+ | 40.6 | ||
| Mussel | Frag 1 | −0.2 | 2.2 ± 0.6 | Frag 1 | −0.2 | 3.8 ± 0.6 |
| January 2011 | Frag 2 | 0.5 | Frag 2 | −2.6 | ||
| Fangar Bay | Frag 3 | 0.4 | Frag 3 | −0.7 | ||
| OYS110115 | [M + H]+ | 0.4 | [M + H]+ | Δppm > 5 ppm | ||
| Oyster | Frag 1 | −0.2 | 5 ± 1 | Frag 1 | Δppm > 5 ppm | ND |
| January 2011 | Frag 2 | 0.3 | Frag 2 | Δppm > 5 ppm | ||
| Fangar Bay | Frag 3 | 2.3 | Frag 3 | Δppm > 5 ppm | ||
| MUS110116 | [M + H]+ | 1.6 | [M + H]+ | 1.3 | ||
| Mussel | Frag 1 | 0.1 | 3.6 ± 0.18 | Frag 1 | 0.5 | 3 ± 1 |
| January 2011 | Frag 2 | −0.1 | Frag 2 | −0.2 | ||
| Fangar Bay | Frag 3 | 0.9 | Frag 3 | −0.1 | ||
| OYS110117 | [M + H]+ | −0.1 | [M + H]+ | Δppm > 5 ppm | ||
| Oyster | Frag 1 | 0.1 | 6.6 ± 0.7 | Frag 1 | Δppm > 5 ppm | ND |
| January 2011 | Frag 2 | −0.1 | Frag 2 | Δppm > 5 ppm | ||
| Fangar Bay | Frag 3 | −0.9 | Frag 3 | Δppm > 5 ppm | ||
| OYS110205 | [M + H]+ | 0.4 | [M + H]+ | Δppm > 5 ppm | ||
| Oyster | Frag 1 | −0.1 | 5.8 ± 0.5 | Frag 1 | Δppm > 5 ppm | ND |
| February 2011 | Frag 2 | 0.1 | Frag 2 | Δppm > 5 ppm | ||
| Fangar | Frag 3 | 1.6 | Frag 3 | Δppm > 5 ppm | ||
| MUS110205 | [M + H]+ | −0.2 | [M + H]+ | 2.2 | ||
| Mussel | Frag 1 | 0.3 | NQ | Frag 1 | 0.5 | 4.1 ± 0.1 |
| February 2011 | Frag 2 | −0.2 | Frag 2 | −1.8 | ||
| Fangar Bay | Frag 3 | 0.9 | Frag 3 | 0.4 | ||
| MUS1027 | [M + H]+ | 0.2 | [M + H]+ | 42.6 | ||
| Mussel | Frag 1 | −0.6 | 3 ± 2 | Frag 1 | −0.5 | 2.2 ± 0.1 |
| February 2011 | Frag 2 | −1.0 | Frag 2 | −1.9 | ||
| Fangar Bay | Frag 3 | 0.3 | Frag 3 | −2.00 | ||
| OYS110208 | [M + H]+ | 0.5 | [M + H]+ | Δppm > 5 ppm | ||
| Oyster | Frag 1 | −0.2 | 4 ± 1 | Frag 1 | Δppm > 5 ppm | ND |
| February 2011 | Frag 2 | 0.1 | Frag 2 | Δppm > 5 ppm | ||
| Fangar | Frag 3 | −1.0 | Frag 3 | Δppm > 5 ppm | ||
| MUS120520 | [M + H]+ | 1.0 | [M + H]+ | −1.1 | ||
| Mussel | Frag 1 | −0.5 | NC | Frag 1 | −0.5 | 39 ± 6 |
| May 2012 | Frag 2 | Δppm > 5 ppm | Frag 2 | −0.7 | ||
| Fangar Bay | Frag 3 | Δppm > 5 ppm | Frag 3 | −0.9 | ||
| MUS120523 | [M + H]+ | −2.1 | [M + H]+ | 0.2 | ||
| Mussel | Frag 1 | −0.1 | 16 ± 1 | Frag 1 | −0.1 | 59 ± 5 |
| May 2012 | Frag 2 | 0.4 | Frag 2 | −0.1 | ||
| Retail market | Frag 3 | −0.1 | Frag 3 | −0.1 | ||
| MUS120524 | [M + H]+ | Δppm > 5 ppm | [M + H]+ | −1.1 | ||
| Mussel | Frag 1 | −1.1 | NC | Frag 1 | −0.5 | 58 ± 2 |
| May 2012 | Frag 2 | Δppm > 5 ppm | Frag 2 | −0.9 | ||
| Fangar Bay | Frag 3 | Δppm > 5 ppm | Frag 3 | −0.9 | ||