Validation of an ultra-high performance liquid chromatography-tandem mass spectrometry method for determination of aflatoxins and ochratoxin A in spices: application to the analysis of samples from the Serbian market
2011
Škrbić, B., Faculty of Technology, Novi Sad (Serbia) | Koprivica, S., Faculty of Technology, Novi Sad (Serbia) | Đurišić-Mladenović, N., Faculty of Technology, Novi Sad (Serbia) | Hajšlová, J., Faculty of Food and Biochemical Technology, Prague (Czech Republic). Institute of Chemical Technology, Department of Food Chemistry and Analysis
The aim of this study was to validate a simple analytical method for determination of the EU-regulated mycotoxins in spices based on the UHPLC-HESI-MS/MS (Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry equipped with heated electrospray ionization source) analysis of crude extracts. Validation of the method was carried out in two different matrices, powdered red pepper and black pepper, representing ones of the most important and favorite spices all over the world. The method was validated by measuring the accuracy, precision, linearity, limits of detection (LOD) and limits of quantification (LOQ). The obtained validation data suggested that the analysis of red pepper crude extracts is indeed feasible and at the same time sensitive enough for determining AFs and OTA levels set in the EU legislation (No. 165/2010 and 105/2010). However, validation parameters for analysis of some mycotoxins in black pepper crude extracts did not comply with the EU regulation, particularly with respect to the recoveries and LODs for AFG1, AFG2 and OTA, due to significant matrix interferences. The validated method has been applied to the analysis of red pepper samples collected from local markets in Novi Sad, capitol of the Vojvodina Province, where the biggest producers of spice in Serbia are located. None of the samples contained mycotoxins in concentration detectable by the applied method.
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