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.

Autore Pugliese

• Nardiello Donatella

Tutti gli autori

• M. Muscarella , M. Iammarino , D. Nardiello , C. Palermo , D. Centonze

Titolo volume/Rivista

TALANTA

Anno di pubblicazione

2012

ISSN

0039-9140

ISBN

Non Disponibile

Numero di citazioni Wos

11

Ultimo Aggiornamento Citazioni

Non Disponibile

Numero di citazioni Scopus

12

Ultimo Aggiornamento Citazioni

Non Disponibile

Settori ERC

Non Disponibile

Codici ASJC

Non Disponibile