In-house method validation, estimating measurement uncertainty and the occurrence of fumonisin B<inf>1</inf> in samples of Brazilian commercial rice

Abstract

Fumonisin B<inf>1</inf> was investigated in samples of rice intended for human consumption, including polished parboiled rice, whole grain rice and whole grain parboiled rice. Until the present, no studies on the occurrence of fumonisin B<inf>1</inf> have been performed on these types of rice that are commercially available in the south-eastern region of Brazil. A careful intralaboratory validation was carried out to demonstrate the fitness-of-purpose of the applied method for determining fumonisin B<inf>1</inf> in the three studied rice types. The performance criteria - selectivity, reliable limits of detection (50μgkg^-1) and quantification (100μgkg^-1), linearity (range 100-2500μgkg^-1), precision (RSD values≤17.0%) and recovery (71.7-112.0 %) were evaluated, and the expanded measurement uncertainty was estimated by using the data obtained from precision and recovery experiments. Matrix-matched calibration standards were employed to quantify the mycotoxin levels in the rice samples, in which the residual normality, homoscedasticity and independence were confirmed. In addition, the measurement uncertainty values are consistent with the maximum acceptable uncertainty established by European Union regulation for analytical methods for controlling mycotoxins in foodstuffs. Among the thirty-one commercial samples of rice analysed in the present study, five samples presented detectable levels of the mycotoxin, and these levels ranged from 64.8 to 163.0μgkg^-1.