粮食及加工品中环境污染物检测方案

面粉中溴酸盐的检测——离子色谱法结合英蓝渗析技术 李涛*，孙焕，陶玲 瑞士万通中国有限公司中心实验室，北京，10085 Bj.lit@metrohm.com.cn 本文建立了基于离子色谱法搭配英蓝渗析技术的针对面粉当中的溴酸盐含量的定量分析方法。分析过程采用等度淋洗方式，并采用电导检测与柱后衍生（碘化法）紫外/可见检测方式串联的检测技术。柱后衍生剂选取硫酸+四水钼酸铵（试剂1）和碘化钾溶液（试剂2）的组合。样品溶解后，在室温条件下超声提取30分钟，随后在6000rpm条件下离心10分钟。样品经英蓝渗析处理后进入离子色谱进行分析。 实验结果表明，在该方法条件下，以实际面粉样品为基质，在50μg/L~250μg/L浓度范围内，溴酸盐的检测具有良好的线性关系（R2=0.9999）与回收率（80%~120%）。 本文对英蓝渗析技术和传统的样品前处理方式进行了比较，结果表明，两种前处理方式均可以得到令人满意的实验的结果，前处理方式对实验结果的影响不显著。但英蓝渗析技术可大大缩短样品前处理过程并较少人力消耗。 Determination of Bromate in Flour using Inline Dialysis and combined Conductivity and UV/Vis Detection after Post-Column Reaction Tao Li*, Huan Sun, Ling Tao Cclab of Metrohm Chian, Beijing, 10085 Bj.lit@metrohm.com.cn Bromate has been analyzed in flour by ion chromatography using Inline Dialysis with isocratic elution and combined conductivity and UV detection after post column reaction (triiodide method) with a solution of sulfuric acid and ammonium-heptamolybdate tetrahydrate (reagent 1) and potassium iodide solution (reagent 2). The sample has been extracted by sonification for 30 minutes at ambient temperature followed by centrifugation for 10 minutes at 6000 rpm. The results showed that, based on the built method, there was a good linearity of bromate in the range of 50μg/L~250μg/L. And the recovery in the same concentration range was in the range of 80% ~120%. The comparison between In-line dialysis and traditional sample preparation was further done in this paper. The results showed that, there was no significant difference between these two sample preparation processes. But the In-line dialysis technique is less time consuming and workforce consuming.