A fast, less expensive, analytical approach with high metrologic reliability was developed to assist an official program for 21 marine biotoxins, monitoring in bivalve mollusks. The simultaneous analysis of lipophilic and hydrophilic marine biotoxins was achieved using a sample preparation protocol based on solid-liquid extraction and low-temperature cleanup, followed by liquid chromatography coupled to tandem mass spectrometry. Samples were extracted with acidified methanol/water (90:10), followed by low-temperature cleanup. Chromatographic separation was obtained using a cyano-bonded silica phase. The mobile phase was composed of water and acetonitrile, with both 0.1% formic acid and 2.5 mmol L-1 ammonium formate. Electrospray ionization was used in both negative and positive modes. The single-laboratory validation approach enabled method performance assessment, and the necessary data to design a model for result expression were yielded. With this purpose, a systematic study of errors and uncertainties was performed. This new analytical approach aimed to minimize the use of highly expensive analytical standards, promoting economic viability to be applied by high-throughput routine laboratories. After its implementation on the Brazilian official monitoring program, positive results near the regulatory limits were obtained, demonstrating the fit for purpose of the method as a surveillance tool.
Keywords: food inspection; hydrophilic toxins; lipophilic toxins; measurement uncertainty; reference methods; seafood analysis.