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Abstract
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. After taking both these factors into account, a recovery of 80% could be achieved. The GC method was used to carry out a survey of retail bread samples in 1989. Bromate was found in all six unwrapped breads analysed (median 35 jig/kg, range 17–317 μg/kg), whilst for 22 wrapped breads, seven were found to contain bromate (median < 12 μg/kg, range < 12–238 μg/kg). A second method of analysis employing inductively coupled plasma‐mass spectrometry (ICP‐MS) was developed which provided independent confirmation of the presence of bromate in these retail samples. The method gave a mean recovery of 71% from five spiked samples and a detection limit of 20 μg/kg. The GC and ICP‐MS methods were compared by performing replicate analyses of a bread sample prepared with bromate‐treated flour. Quantitative agreement between the two techniques was good. The precision of the ICP‐MS technique (CV 12%) proved better than that found for the GC method (CV 18%). The Potassium Bromate (Prohibition as a Flour Improver) Regulation 1990 came into force on 1 April 1990 (Statutory Instrument 1990 Number 399). A second survey of those brands of bread which had previously been found to contain bromate was carried out in 1992. All samples contained less than the detection limit of 12 μg potassium bromate/kg flour.