摘要
建立了面米制品及膨化食品中溴形态的微波革取前处理方式，采用高效液相色谱（HPLC）和电感耦合等离子体质谱（ICP—MS）联用分析技术。以微波萃取溴酸盐及溴化物，用C18固相萃取小柱净化和0．45μm水相滤膜过滤，以PA-100（250mm×4mm）阴离子色谱柱分离溴形态，50mmol／L硝酸铵为流动相，流速1．0mL／min；进样体积100μL，HPLC—ICP—MS测定。在2．0～50μg／L范围内呈现良好的线性关系，溴酸盐和溴离子检出限为0．64、0．80μg／L，方法回收率89．0％～108％，精密度0．87％-5．80％。结果表明，该方法快速、简便、灵敏度高、干扰少，尤其适用于检测基体复杂的膨化食品中痕量的溴酸钾含量，克服了采用GB／T20188--2006离子色谱法检测膨化食品中溴酸盐含量时可能存在的假阳性，为食品中溴酸盐检测提供了一种可靠、科学和准确的确证方法。
HPLC-ICP-MS in conjunction with microwave extraction was developed to analyse the trace bromine speciation in flour and rice products and puffed food. The sample was microwave extracted by water and purified with C18 SPE and filtrated by 0.45 tim membrane filters. BrO3- and Br-were separated on a DIONEX CarboPac PA-100 （250 mm×4 mm） column with 50 mmol Ammonium nitrate as mobile phase at 1.0 mL/min with 100 pL injection volume, then detected by ICP-MS. This method achieved practical quantitation limits for the oxyhalides bromate of 0.64 μg/L, while Bf 0.80 μg/L. BrO3 and Br showed goodlinear relationship in the range of 2 to 50 μg/L. The recoveries and precision of the method for BrO3- and Br- were 89.0%~108% and 0.87%~5.80%, respectively. The results show that this method is rapid, simple, sensitive, less interference, especially for the detection of complex puffed food matrix trace levels of bromate, overcomeing the false positive detection of bromate using GB/T 20188--2006. This level of measurement allows for the accurate assessment of BrOw and Br in puffing food.
出处
《食品科技》
CAS
北大核心
2014年第5期282-287,共6页
Food Science and Technology
基金
浙江省国境安全检验检疫科技创新服务平台项目(2006C17014)
浙江出入境检验检疫局科技项目(ZK201246)
