A sensitive and selective analytical method was developed for the quantitative determination of fumonisins B1 and B2 in maize-based foods for direct human consumption. The method, based on highperformance liquid chromatography and fluorescence detection, presents a rapid and automated on-line post-column derivatization, performed with o-phtalaldehyde and N,N-dimethyl-2-mercaptoethylamine. Several factors affecting the separation and detection of fumonisins were investigated, including mobile phase composition, column features, derivatization agent flow-rate and both the excitation and the emission wavelengths. Optimal fluorescence detection was obtained by using a exc of 343 nm and a em of 445 nm. Under the optimized experimental conditions, a complete separation of fumonisinswas obtained in less than 13 min by using a C18 column and a gradient elution at 0.8 mL/min with methanol and 0.1M phosphate buffer at pH 3.15. The limits of detection for FB1 and FB2 were 4 and 5g/L corresponding to 5 and 6g/kg in matrix. Each fumonisin was determined in the range 40–320g/L that correspond to 50–400g/kg in matrix. The necessary requirements for accuracy, reproducibility and sensitivity were fulfilled and recovery values ranged from87 to 94% for FB1 and from70 to 75% for FB2 in cornflake samples at three fortification levels in the range 100–300 g/kg. The potential of this method, combined with a simple clean-up procedure, was assessed by the measurements of FB1 and FB2 in maize-based products, such as maize flour, “polenta”, tortillas and cookies.
Development of a new analytical method for the determination of fumonisins B1 and B2 in food products based on high performance liquid chromatography and fluorimetric detection with post-column derivatization
NARDIELLO, DONATELLA;PALERMO, CARMEN;CENTONZE, DIEGO
2008-01-01
Abstract
A sensitive and selective analytical method was developed for the quantitative determination of fumonisins B1 and B2 in maize-based foods for direct human consumption. The method, based on highperformance liquid chromatography and fluorescence detection, presents a rapid and automated on-line post-column derivatization, performed with o-phtalaldehyde and N,N-dimethyl-2-mercaptoethylamine. Several factors affecting the separation and detection of fumonisins were investigated, including mobile phase composition, column features, derivatization agent flow-rate and both the excitation and the emission wavelengths. Optimal fluorescence detection was obtained by using a exc of 343 nm and a em of 445 nm. Under the optimized experimental conditions, a complete separation of fumonisinswas obtained in less than 13 min by using a C18 column and a gradient elution at 0.8 mL/min with methanol and 0.1M phosphate buffer at pH 3.15. The limits of detection for FB1 and FB2 were 4 and 5g/L corresponding to 5 and 6g/kg in matrix. Each fumonisin was determined in the range 40–320g/L that correspond to 50–400g/kg in matrix. The necessary requirements for accuracy, reproducibility and sensitivity were fulfilled and recovery values ranged from87 to 94% for FB1 and from70 to 75% for FB2 in cornflake samples at three fortification levels in the range 100–300 g/kg. The potential of this method, combined with a simple clean-up procedure, was assessed by the measurements of FB1 and FB2 in maize-based products, such as maize flour, “polenta”, tortillas and cookies.I documenti in IRIS sono protetti da copyright e tutti i diritti sono riservati, salvo diversa indicazione.
