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

• Published in: Food chemistry 2024-09, Vol.451, p.139416-139416, Article 139416
• Main Authors: El-Bahar, Amira A. Abdulrahman, Shendy, Amr H., Aboalhassen, Alaa El-Dean Fathy Ahmed, Gomaa, Ahmed M., Ismail, Eman H.
• Format: Article
• Language: English
• Subjects: Bakery products; Baladi bread; Bromate additive; consumer protection; Flour; food chemistry; LC-ESI-MS/MS; mass spectrometry; Solid-liquid extraction; solvents
• ISSN: 0308-8146; 1873-7072
• DOI: 10.1016/j.foodchem.2024.139416

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 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.