title: Optimized and validated high-performance liquid chromatography method for the determination of deoxynivalenol and aflatoxins in cereals.
abstract: A simple, sensitive and accurate analytical method was optimized and developed for the determination of deoxynivalenol and aflatoxins in cereals intended for human consumption using high-performance liquid chromatography with diode array and fluorescence detection and a photochemical reactor for enhanced detection. A response surface methodology, using a fractional central composite design, was carried out for optimization of the water percentage at the beginning of the run (X1, 80-90%), the level of acetonitrile at the end of gradient system (X2, 10-20%) with the water percentage fixed at 60%, and the flow rate (X3, 0.8-1.2 mL/min). The studied responses were the chromatographic peak area, the resolution factor and the time of analysis. Optimal chromatographic conditions were: X1 = 80%, X2 = 10%, and X3 = 1 mL/min. Following a double sample extraction with water and a mixture of methanol/water, mycotoxins were rapidly purified by an optimized solid-phase extraction protocol. The optimized method was further validated with respect to linearity (R(2) >0.9991), sensitivity, precision, and recovery (90-112%). The application to 23 commercial cereal samples from Greece showed contamination levels below the legally set limits, except for one maize sample. The main advantages of the developed method are the simplicity of operation and the low cost.
authors.affiliation: Department of Food Technology, Alexander Technological Educational Institute of Thessaloniki (ATEITh), Greece.|Hellenic Agricultural Organization - Demeter, Plant Breeding and Genetic Resources Institute, Greece.
authors.forename: Adriana
authors.initials: A
authors.lastname: Skendi
authors.affiliation: Hellenic Agricultural Organization - Demeter, Plant Breeding and Genetic Resources Institute, Greece.
authors.forename: Maria N
authors.initials: MN
authors.lastname: Irakli
authors.affiliation: Department of Food Technology, Alexander Technological Educational Institute of Thessaloniki (ATEITh), Greece.
authors.forename: Maria D
authors.initials: MD
authors.lastname: Papageorgiou
mesh_terms: D000348:Aflatoxins / Q000032:analysis*; D002851:Chromatography, High Pressure Liquid; D002523:Edible Grain / Q000737:chemistry*; D014255:Trichothecenes / Q000032:analysis*
chemical_list: D000348:Aflatoxins; D014255:Trichothecenes; C007262:deoxynivalenol
keywords: Aflatoxins; Cereals; Deoxynivalenol; Response surface methodology; Solid-phase extraction