Abstract
In this study, the alkaline ashing and derivatization conditions of our previous gas chromatographic determination of total bromine using 3-pentanone derivatization were improved for the analysis of agricultural products.A 2g sample (for cereals and beans), or a 5g sample (for vegetables and fruits) was ashed with 5ml of 5% potassium hydroxide in ethanol-water (1:1) mixture at 550°C for 5 hours. Bromide in a water extract of the ash residue was converted into the bromo derivative of 3-pentanone (BP), and then determined by capillary gas chromatography with an electron-capture detector. The addition of sulfamic acid to a water extract increased the peak height of BP, and suppressed the formation of the chloro derivative of 3-pentanone.Recoveries of bromide from agricultural products spiked at 5μg/g ranged from 87.2 to 96.8%. The detection limits were 0.05μg/g for cereals and beans, and 0.02μg/g for vegetables and fruits.
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