Ion Chromatography–High-Resolution Mass Spectrometry Method for the Determination of Bromide Ions in Cereals and Legumes: New Scenario for Global Food Security

Abstract

The new scenario for global food production and supply is decidedly complex given the current forecast of an increase in food fragility due to international tensions. In this period, exports from other parts of the world require different routes and treatments to preserve the food quality and integrity. Fumigation is a procedure used for the killing, removal, or rendering infertile of pests, with serious dangers to human health. The most-used fumigants are methyl bromide and ethylene dibromide. It is important to bear in mind that the soil may contain bromide ions naturally or from anthropogenic source (fertilizers and pesticides that contain bromide or previous fumigations). Different methods (titrimetric, spectrophotometric, and fluorometric approaches) are available to rapidly determine the amount of bromide ion on site in the containers, but these are non-specific and with high limits of quantification. The increasing interest in healthy food, without xenobiotic residues, requires the use of more sensitive, specific, and accurate analytical methods. In order to help give an overview of the bromide ion scenario, a new, fast method was developed and validated according to SANTE 11312/2021. It involves the determination of bromide ion in cereals and legumes through ion chromatography–Q-Orbitrap. The extraction was performed by the QuPPe method, but some modifications were applied based on the matrix. The method described here was validated at four different levels. Recoveries were satisfactory and the mean values ranged between 99 and 106%, with a relative standard deviation lower than 3%. The linearity in the matrix was evaluated to be between 0.010 and 2.5 mg kg−1, with a coefficient of determination (R2) of 0.9962. Finally, the proposed method was applied to different cereals and legumes (rice, wheat, beans, lentils pearled barley, and spelt) and tested with satisfactory results in EUPT-SMR16 organized by EURL.