Coupling of a streamlined solid-liquid extraction protocol with LC-ESI-MS/MS for the regular oversight of illegal bromate additive use: An accurate and sensitive determination method in preliminary and bakery products.

A reliable solid-liquid extraction protocol coupled with liquid chromatography-electrospray ionization-tandem mass spectrometry in the negative-ion mode was developed and validated for illegal bromate determination in preliminary and bakery products. Crude and dried-treated samples were directly extracted with acetonitrile-water (4:1, v/v). Bromate was determined using a Phenomenex Synergi™ Polar reversed-phase column and MS/MS under multiple reaction monitoring. The chosen solvent efficiently extracted bromate with all applied extraction-assisting techniques (p > 0.05). Although this assay avoids cleanup procedures, matrix effect of <−11% was achieved. Rapid bromate separation in only 8 min was attained by a reversed-phase column. In both commodities, linearity range, R2, recovery%, repeatability, intermediate precision, LOD and LOQ results were 0.05–100 ng mL−1, >0.9999, 88.6–103%, 2.93–9.80% and 9.64–10.10%, 0.015 μg kg−1 and 0.05 μg kg−1, respectively. Out of 288 tested real samples, 13.9% of violations were observed. This high-sensitivity protocol offers effective oversight and consumer protection. • Bromate was analyzed with a simple solid-liquid extraction method in bakery products. • Univariate analyses helped optimal selection of sample processing procedures. • Reversed-phase chromatography enabled rapid, accurate, and selective bromate testing. • Superior method sensitivity ensured effective bromate illegal use oversight. • High violation rates of 13.9% recall a national bromate monitoring program. [ABSTRACT FROM AUTHOR]