title: A fully automated method for simultaneous determination of aflatoxins and ochratoxin A in dried fruits by pressurized liquid extraction and online solid-phase extraction cleanup coupled to ultra-high-pressure liquid chromatography-tandem mass spectrometry.
abstract: According to current demands and future perspectives in food safety, this study reports a fast and fully automated analytical method for the simultaneous analysis of the mycotoxins with high toxicity and wide spread, aflatoxins (AFs) and ochratoxin A (OTA) in dried fruits, a high-risk foodstuff. The method is based on pressurized liquid extraction (PLE), with aqueous methanol (30%) at 110 °C, of the slurried dried fruit and online solid-phase extraction (online SPE) cleanup of the PLE extracts with a C18 cartridge. The purified sample was directly analysed by ultra-high-pressure liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) for sensitive and selective determination of AFs and OTA. The proposed analytical procedure was validated for different dried fruits (vine fruit, fig and apricot), providing method detection and quantification limits much lower than the AFs and OTA maximum levels imposed by EU regulation in dried fruit for direct human consumption. Also, recoveries (83-103%) and repeatability (RSD < 8, n = 3) meet the performance criteria required by EU regulation for the determination of the levels of mycotoxins in foodstuffs. The main advantage of the proposed method is full automation of the whole analytical procedure that reduces the time and cost of the analysis, sample manipulation and solvent consumption, enabling high-throughput analysis and highly accurate and precise results.
authors.affiliation: Dipartimento di Farmacia, Università di Salerno, Via Giovanni Paolo II 132, 84084, Fisciano, SA, Italy.
authors.forename: Luca
authors.initials: L
authors.lastname: Campone
authors.forename: Anna Lisa
authors.initials: AL
authors.lastname: Piccinelli
authors.forename: Rita
authors.initials: R
authors.lastname: Celano
authors.forename: Mariateresa
authors.initials: M
authors.lastname: Russo
authors.forename: Alberto
authors.initials: A
authors.lastname: Valdés
authors.forename: Clara
authors.initials: C
authors.lastname: Ibáñez
authors.forename: Luca
authors.initials: L
authors.lastname: Rastrelli
mesh_terms: D000348:Aflatoxins / Q000032:analysis*; D001331:Automation; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D005504:Food Analysis; D005506:Food Contamination / Q000032:analysis; D005638:Fruit / Q000737:chemistry*; D006863:Hydrogen-Ion Concentration; D009793:Ochratoxins / Q000032:analysis*; D052616:Solid Phase Extraction / Q000379:methods*; D053719:Tandem Mass Spectrometry / Q000379:methods*; D013696:Temperature
chemical_list: D000348:Aflatoxins; D009793:Ochratoxins; C025589:ochratoxin A