Multiclass analysis of mycotoxins in biscuits by high performance liquid chromatography–tandem mass spectrometry. Comparison of different extraction procedures

• An LC/ESI-MS/MS method for the determination of mycotoxins in biscuits.
• Different sample preparations were evaluated.
• Samples were extracted and cleaned-up using graphitized carbon black.
• Quantification limits were lower than maximum permitted levels.

A sensitive, simple and rapid method for the simultaneous determination of 19 mycotoxins in biscuits (a dry matrix containing cereals and egg) has been developed using high performance liquid chromatography coupled to tandem mass spectrometry with electrospray source working in both positive and negative mode.Due to the matrix complexity and the high amount of contaminants, a solid phase extraction method using graphitized carbon black was optimized for an effective clean-up step. Accuracy was carried out in the selected matrix using blank samples spiked at three analyte concentrations. Recoveries between 63 and 107% and relative standard deviations lower than 12% were obtained. For all considered mycotoxin classes, i.e. thricotecenes A and B, zearalenone and its metabolites, fumonisins, ochratoxin A, enniatins and their structurally related beauvericin, the method was validated in terms of linearity, recovery, matrix effect, precision, limit of detection and limit of quantification. Matrix-matched calibration was used for quantification purposes, in order to compensate for matrix effect. The coefficients of determination obtained were in the range of 0.9927–1. The limits of quantification, ranging from 0.04 μg kg−1 for enniatin B1 to 80.2 μg kg−1 for nivalenol, were always lower than maximum permitted levels for every regulated mycotoxin by the current European legislation.