K. Himata et al., DETERMINATION OF BROMATE IN BREAD BY CAPILLARY GAS-CHROMATOGRAPHY WITH A MASS DETECTOR (GC MS), Food additives and contaminants, 11(5), 1994, pp. 559-569
A sensitive method was developed for the determination of bromate in b
read by capillary gas chromatography with a mass detector (GC/MS). Bro
mate was extracted with water from bread samples. After centrifigation
, the supernatant was filtered and Cl- was removed by an OnGuard-Ag ca
rtridge column. The mixture was absorbed on a DEA solid phase extracti
on column and washed with water. Bromate was then eluted with 3 M pota
ssium chloride solution. Two ml of 4 x 10(-3) M styrene monomer soluti
on (washed with 1% sodium hydroxide solution before use), 1 ml 0.01 M
potassium bromide solution and 1 ml sulphuric acid were added to the e
luent and shaken vigorously. The styrene bromo derivative momethyl-ben
zenemethanol[2-bromo-1-phenylethanol]) was extracted with 2 ml n-hexan
e, and determined by GC/MS. Recoveries of bromate from breads were in
the range 91.3-98.1% (0.03-0.50 mug/g), and the limit of detection was
0.03 mug/g. Pullman and open top types of white bread, produced by a
sponge and dough method and a short process method respectively, were
prepared in our laboratory for measurement of residual bromate. When 3
0 mug/g or less bromate as HBrO3 (pullman type), and 75 mug/g bromate
or less as KBrO3 (open top type), was added to flour, no residual brom
ate was detected in either type of bread.