| 摘要: | Marine shellfish toxins are seafood safety problems of global concern. Herein the analysis of six shellfish toxins, regulated by European Union, with one single run by LC-MS/MS with acidic mobile phase was developed. After 80% methanol extraction of the shellfish toxins, the crude extract was subjected to HLB SPE cleanup before LC-MS/MS analysis. The method was validated according to Commission Decision 2002/657/EC. For azaspiracid-1 (AZA1), domoic acid (DA), dinophysistoxin-1 (DTX1), okadaic acid (OA), pectenotoxin-2 (PTX2), and yessotoxin (YTX) toxins the recovery rate was 99.4, 92.7, 114.1, 90.2, 115.2 and 87.8%, respectively. The intra-day relative standard deviation (RSD) was less than 5% for all of the shellfish toxins except DA. The inter-day RSD was less than 5% for AZA1, DTX1, PTX2, YTX, 7.85% for DA, and 14.63% for OA. The decision limit (CCα) and detection capability (CCβ) for AZA1 were 13.6 and 14.8 ppb; for DA they were 1883 and 2051 ppb; DTX1 12.3 and 13.4 ppb; OA 8.0 and 8.7 ppb; PTX2 12.1 and 13.2 ppb; YTX 36.9 and 40.1 ppb. |
