Kawasaki Yoko, Kubota Hiroki, Yomota Chikako, Maitani Tamio
National Institute of Health Sciences: 1-18-1, Kamiyoga, Setagaya-ku, Tokyo 158-8501, Japan.
Shokuhin Eiseigaku Zasshi. 2002 Aug;43(4):221-4. doi: 10.3358/shokueishi.43.221.
An effective clean-up procedure was developed to determine trace levels of bromate in bread by high-performance liquid chromatography with post-column flow reactor detection. Bromate was extracted from bread with deionized pure water. After centrifugation, the supernatant was filtered through a paper filter. The filtrate was filtered through a 0.2 micron nylon filter and chloride ion was removed by an IC-SP M Ag cartridge column or On-Guard Ag cartridge column. The eluate was applied to an Oasis MAX anion exchange cartridge column. The column was washed with 20% acetic acid and water. Bromate was then eluted with 0.5% sodium nitrate solution. The eluate was determined by HPLC with post column flow reactor detection. The method had a quantitation limit of 2 ng/g in bread products. Recoveries of bromate from bread ranged from 68 to 72% at a spiked bromate level of 2-10 ng/g.
开发了一种有效的清理程序,通过柱后流动反应器检测的高效液相色谱法测定面包中的痕量溴酸盐。用去离子纯水从面包中提取溴酸盐。离心后,上清液通过纸质过滤器过滤。滤液通过0.2微米尼龙过滤器过滤,氯离子用IC-SP M Ag柱或On-Guard Ag柱除去。洗脱液应用于Oasis MAX阴离子交换柱。该柱先用20%乙酸和水冲洗。然后用0.5%硝酸钠溶液洗脱溴酸盐。洗脱液通过柱后流动反应器检测的高效液相色谱法测定。该方法在面包产品中的定量限为2 ng/g。在2-10 ng/g的加标溴酸盐水平下,面包中溴酸盐的回收率为68%-72%。