Multivariate optimization of a solid phase extraction method for ochratoxin A in wine samples prior to UPLC-MS/MS

VICTOR VANDELL, L. MARIÑO REPIZO, S. CERUTTI, J. RABA, F. KERO, W. HARTSOCK

Chicago, Illinois

Congreso; AOAC 127th Annual Meeting & Exposition; 2014

AOAC International

Recent trends in regulatory programs for food safety have focused on the emerging threat of mycotoxins in foods. Ochratoxin A (OTA) is a toxic metabolite produced by several fungi of the genera Aspergillus and Penicillium and commonly found in red wine and other foodstuffs. OTA is more frequently detected in red wines than in rosé and white wines. Due to a wide range of its toxic effects in humans and animals, OTA needs to be monitored. For this reason, to protect consumer health, the European Commission has established a maximum permitted level (ML) of 2 μg L-1 of OTA in wine. Due to OTA?s properties and the fact that it is present at low concentrations, extraction and determination in wine samples constitutes an analytical challenge. Immunoaffinity column samples clean-up associated to liquid chromatography and fluorescence detection is method of choice for OTA quantification in wine. In this work, red wine samples were prepared leveraging new advances in solid phase extraction (SPE) column technology (ISOLUTE® Myco) prior to analysis by UPLC-MS/MS. Strategies employing statistical design of experiments demonstrated to minimize heuristic efforts associated with analytical method development. The methodology was validated according to the EU normative and the obtained figures of merit are compatible with the ML established.