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建立了面米制品及膨化食品中溴形态的微波萃取前处理方式,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(250 mm×4 mm)阴离子色谱柱分离溴形态,50 mmol/L硝酸铵为流动相,流速1.0 mL/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/T 20188—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。
A pre-treatment method of microwave extraction of bromine in noodle products and puffed food was established. The analytical techniques were analyzed by high performance liquid chromatography (HPLC) and inductively coupled plasma mass spectrometry (ICP-MS). The bromates and bromides were extracted by microwave and purified by C18 solid phase extraction cartridges and filtered with 0.45μm aqueous phase. The bromine was separated on a PA-100 (250 mm × 4 mm) anion chromatographic column and 50 mmol / L nitric acid Ammonium as mobile phase, flow rate 1.0 mL / min; injection volume 100 μL, HPLC-ICP-MS determination. The linear range was 2.0-50μg / L. The detection limits of bromate and bromide were 0.64,0.80μg / L. The recoveries were 89.0% -108% and the precision was 0.87% -5.80%. The results show that the method is rapid, simple, sensitive and less interference, especially for the detection of trace amount of potassium bromate in puffed food with complex matrix. It overcomes the problem of using bromate in GB / T 20188-2006 ion- The false positives that may be present in the content provide a reliable, scientific and accurate confirmation of bromate in foods.