LC-MS/MS method for the detection of multiple classes of shellfish toxins

Abstract

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 (CC_α) and detection capability (CC_β) 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.