The implementation of liquid chromatography tandem mass spectrometry for the official control of lipophilic toxins in seafood: Single-laboratory validation under four chromatographic conditions
| Autor: | Jorge Diogène, María García-Altares, P. de la Iglesia |
|---|---|
| Přispěvatelé: | IRTA. Recerca i Tecnologia Agroalimentàries |
| Rok vydání: | 2013 |
| Předmět: |
Food Safety
Cromatografia líquida Context (language use) Reference laboratory Mass spectrometry Sensitivity and Specificity Biochemistry Analytical Chemistry Tandem Mass Spectrometry Liquid chromatography–mass spectrometry Animals media_common.cataloged_instance European Union European union media_common Chromatography Elution Chemistry Methanol Organic Chemistry Reproducibility of Results General Medicine Hydrogen-Ion Concentration Bivalvia Toxines marines Espectrometria de masses Seafood Sea Urchins Linear Models Marine Toxins Aquaculture industry Hydrophobic and Hydrophilic Interactions Chromatography Liquid |
| Zdroj: | RECERCAT (Dipòsit de la Recerca de Catalunya) Recercat. Dipósit de la Recerca de Catalunya instname |
| ISSN: | 0021-9673 |
| DOI: | 10.1016/j.chroma.2012.12.021 |
| Popis: | We performed a comprehensive study to assess the fit for purpose of four chromatographic conditions for the determination of six groups of marine lipophilic toxins (okadaic acid and dinophysistoxins, pectenotoxins, azaspiracids, yessotoxins, gymnodimine and spirolides) by LC–MS/MS to select the most suitable conditions as stated by the European Union Reference Laboratory for Marine Biotoxins (EURLMB). For every case, the elution gradient has been optimized to achieve a total run-time cycle of 12 min. We performed a single-laboratory validation for the analysis of three relevant matrices for the seafood aquaculture industry (mussels, pacific oysters and clams), and for sea urchins for which no data about lipophilic toxins have been reported before. Moreover, we have compared the method performance under alkaline conditions using two quantification strategies: the external standard calibration (EXS) and the matrix-matched standard calibration (MMS). Alkaline conditions were the only scenario that allowed detection windows with polarity switching in a 3200 QTrap mass spectrometer, thus the analysis of all toxins can be accomplished in a single run, increasing sample throughput. The limits of quantification under alkaline conditions met the validation requirements established by the EURLMB for all toxins and matrices, while the remaining conditions failed in some cases. The accuracy of the method and the matrix effects where generally dependent on the mobile phases and the seafood species. The MMS had a moderate positive impact on method accuracy for crude extracts, but it showed poor trueness for seafood species other than mussels when analyzing hydrolyzed extracts. Alkaline conditions with EXS and recovery correction for OA were selected as the most proper conditions in the context of our laboratory. This comparative study can help other laboratories to choose the best conditions for the implementation of LC–MS/MS according to their own necessities. |
| Databáze: | OpenAIRE |
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