An analytical procedure was developed to measure bromate residues in baked goods using a sequence of clean‐up procedures followed by high performance liquid chromatography (HPLC) with a post‐column reaction for oxidants. Deionized water was used to extract bromate from bread samples. The extract was treated with a C‐18 solid phase extraction column to remove lipids, a cation exchange column with the silver cation to remove chloride, and an ultrafiltration membrane to remove proteins.

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The development and application of two methods for determining bromate in bread are described. A gas chromatographic (GC) method which relied on the formation of a volatile derivative of bromate gave a detection limit of 12 μg/kg. Duplicate analyses agreed well but recovery from breads spiked with bromate were low and averaged 30% for brown bread and 42% for white bread. Further studies indicated that this was caused by the derivatization reaction being suppressed by components of the sample and reagents used in their preparation.

A sensitive method was developed for the determination of bromate in bread by capillary gas chromatography with a mass detector (GC/MS). Bromate was extracted with water from bread samples. After centrifugation, the supernatant was filtered and Cl− was removed by an OnGuard‐Ag cartridge column.

Potassium bromate (KBrO3) is an oxidizing agent that has been used as a food additive, mainly in the bread-making process. Although adverse effects are not evident in animals fed bread-based diets made from flour treated with KBrO3, the agent is carcinogenic in rats and nephrotoxic in both man and experimental animals when given orally. It has been demonstrated that KBrO3 induces renal cell tumors, mesotheliomas of the peritoneum, and follicular cell tumors of the thyroid.