title: Determination of deoxynivalenol and nivalenol by liquid chromatography and fluorimetric detection with on-line chemical post-column derivatization.
abstract: A rapid, sensitive and selective analytical method was developed for the quantitative determination of deoxynivalenol (DON) and nivalenol (NIV) in cereals intended for human and animal consumption. The method, based on liquid chromatography and fluorescence detection, involves an automated 2 channel post-column derivatization, performed with sodium hydroxide, methyl acetoacetate and ammonium acetate. The chromatographic separation was accomplished using a C18 column eluted in isocratic mode with a mixture of 0.01% acetic acid and acetonitrile. Optimal fluorescence detection was obtained by an excitation and emission wavelength of 360 nm and 470 nm, respectively. The sample preparation required a rapid extraction of mycotoxins with water and a purification step by hydrophilic-lipophilic balance column clean-up. Under the optimized experimental conditions, a complete separation of DON and NIV was obtained in less than 20 min. The on-line post-column derivatization ensures excellent results in terms of simplicity and sensitivity, with limits of detection down to 0.014 mg/kg. The proposed method was extensively validated and the analytical performances of linearity (correlation coefficient of 0.9998), selectivity, precision (intra-day precision lower than 8%) and recovery (ranging from 89% to 101%) were evaluated, demonstrating the method feasibility in accurate confirmation analyses.
authors: Istituto Zooprofilattico Sperimentale della Puglia e della Basilicata, Via Manfredonia 20, 71100 Foggia, Italy.
authors: Marilena
authors: M
authors: Muscarella
authors: Marco
authors: M
authors: Iammarino
authors: Donatella
authors: D
authors: Nardiello
authors: Carmen
authors: C
authors: Palermo
authors: Diego
authors: D
authors: Centonze
mesh_terms: D002138:Calibration; D056148:Chromatography, Reverse-Phase / Q000379:methods*; D002523:Edible Grain / Q000737:chemistry; D005470:Fluorometry / Q000379:methods*; D005504:Food Analysis / Q000379:methods*; D006801:Humans; D015203:Reproducibility of Results; D014255:Trichothecenes / Q000032:analysis* / Q000302:isolation & purification
chemical_list: D014255:Trichothecenes; C038405:nivalenol; C007262:deoxynivalenol