title: Multiclass analysis of mycotoxins in biscuits by high performance liquid chromatography-tandem mass spectrometry. Comparison of different extraction procedures.
abstract: 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 0.04μgkg(-1) for enniatin B1 to 80.2μgkg(-1) for nivalenol, were always lower than maximum permitted levels for every regulated mycotoxin by the current European legislation.
authors.affiliation: Department of Chemistry, "La Sapienza" University of Rome, Piazzale Aldo Moro 5, 00185 Rome, Italy.
authors.forename: Anna Laura
authors.initials: AL
authors.lastname: Capriotti
authors.affiliation: Department of Chemistry, "La Sapienza" University of Rome, Piazzale Aldo Moro 5, 00185 Rome, Italy.
authors.forename: Chiara
authors.initials: C
authors.lastname: Cavaliere
authors.affiliation: Department of Chemistry, "La Sapienza" University of Rome, Piazzale Aldo Moro 5, 00185 Rome, Italy. Electronic address: patrizia.foglia@uniroma1.it.
authors.forename: Patrizia
authors.initials: P
authors.lastname: Foglia
authors.affiliation: Department of Chemistry, "La Sapienza" University of Rome, Piazzale Aldo Moro 5, 00185 Rome, Italy.
authors.forename: Roberto
authors.initials: R
authors.lastname: Samperi
authors.affiliation: Department of Chemistry, "La Sapienza" University of Rome, Piazzale Aldo Moro 5, 00185 Rome, Italy.
authors.forename: Serena
authors.initials: S
authors.lastname: Stampachiacchiere
authors.affiliation: Department of Chemistry, "La Sapienza" University of Rome, Piazzale Aldo Moro 5, 00185 Rome, Italy.
authors.forename: Salvatore
authors.initials: S
authors.lastname: Ventura
authors.affiliation: Department of Chemistry, "La Sapienza" University of Rome, Piazzale Aldo Moro 5, 00185 Rome, Italy.
authors.forename: Aldo
authors.initials: A
authors.lastname: Laganà
mesh_terms: D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D009183:Mycotoxins / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*
chemical_list: D009183:Mycotoxins
keywords: Biscuits; Cereal-egg products; Liquid-chromatography; Mass spectrometry; Mycotoxins