Multi-mycotoxin analysis in eggs using a QuEChERS-based extraction procedure and ultra-high-pressure liquid chromatography coupled to triple quadrupole mass spectrometry

Abstract

A reliable and rapid method has been developed for the determination of 10 mycotoxins (beauvericin, enniatin A, A1, B1, citrinin, aflatoxin B1, B2, G1, G2 and ochratoxin A) in eggs at trace levels. Ultra-high-pressure liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) has been used for the analysis of these compounds in less than 7 min. Mycotoxins have been extracted from egg samples using a QuEChERS-based extraction procedure (Quick, Easy, Cheap, Effective, Rugged and Safe) without applying any further clean-up step. Extraction, chromatographic and detection conditions were optimised in order to increase sample throughput and sensitivity. Matrix-matched calibration was used for quantification. Blank samples were fortified at 10, 25, 50 and 100 μg kg −1, and recoveries ranged from 70% to 110%, except for ochratoxin A and aflatoxin G1 at 10 μg kg −1, and aflatoxin G2 at 50 μg kg −1. Relative standard deviations were lower than 25% in all the cases. Limits of detection ranged from 0.5 μg kg −1 (for aflatoxins B1, B2 and G1) to 5 μg kg −1 (for enniatin A, citrinin and ochratoxin A) and limits of quantification ranged from 1 μg kg −1 (for aflatoxins B1, B2 and G1) to 10 μg kg −1 (for enniatin A, citrinin and ochratoxin A). Seven samples were analyzed and aflatoxins B1, B2, G1, G2, and beauvericin were detected at trace levels.