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In-house validation of an LC-MS/MS method for the determination of lipophilic toxins in shellfish species typically tested in the United Kingdom

Project Code: FS235004

14/12/2011

During periods of cultivation, edible shellfish may become contaminated by naturally occurring toxins derived from certain marine algae. One family of these chemicals is the fat-soluble (lipophilic) toxins. Some lipophilic toxins cause severe gastrointestinal disorders in humans following consumption of shellfish contaminated above regulated levels.

The refined method provides an efficient, automated, multi-toxin approach which combines an effective extraction procedure with the specificity of LC-MS/MS analysis, allowing for specific identification and more precise quantification of the range of lipophilic toxins encountered in UK commercially significant shellfish species. It demonstrates many advantages over the former EU reference Mouse bioassay (MBA) method, which although is able to respond to the presence of marine lipophilic toxins, can present ‘false’ results (due to interference from co-extracted shellfish matrix compounds) and is not able to provide any quantitative information on toxin concentrations or specifically identify different toxins or toxin compounds.

The refined method proved particularly sensitive for PTX, AZA and YTX toxins and concentrations as low as 3-11% of the EU regulatory limits were achieved satisfactorily from a range of shellfish species commonly produced by the UK’s shellfish industry.

During inter-laboratory studies, method performance was found to be comparable with other LC-MS/MS techniques applied in laboratories across Europe that monitor similar marine lipophilic toxins. Valuable information regarding the negative (biasing) effects of shellfish extracts on toxin measurements during sample analysis was gained from these studies. Transferring the method to a new, state-of-the-art, ‘fast’ LC-MS/MS instrument reduced sample analysis time by 70% ensuring the technique is responsive to meeting the high demands of shellfish monitoring programmes. Additionally, lower toxin concentrations could be confidently determined. With the advantages of high sensitivity, toxin identification, confirmation and quantitation, the validated method is practical and fit-for-purpose. It provides a suitable replacement for the animal assay and recommendations are made for its implementation in the UK biotoxin statutory monitoring programmes.

Final report

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