ICP-MS法测定食品级壳聚糖中的微量杂质元素

发布时间：2018-01-12 17:33

本文关键词：ICP-MS法测定食品级壳聚糖中的微量杂质元素　出处：《光谱学与光谱分析》2016年08期 　论文类型：期刊论文

【摘要】：建立了电感耦合等离子体质谱(ICP-MS)法直接测定食品级壳聚糖中杂质元素的分析方法。壳聚糖用3%的柠檬酸溶解并加入低浓度盐酸后,采用ICP-MS法直接测定其中的Be,Na,Mg,K,Ca,Ti,V,Cr,Mn,Fe,Co,Ni,Cu,Zn,As,Cd,Sn,Sb,Hg,Pb等20种杂质元素。盐酸的使用有效地改善了元素的稳定性,尤其是Hg和Sn。选择动态反应池(DRC)技术消除了氯离子干扰以及其他质谱干扰,采用基体匹配法并通过加入Sc,Y,In,Bi内标元素混合溶液补偿了样品传输效率的差异以及有机溶剂蒸发速率的影响。在选定的工作条件下,20种元素的标准曲线方程具有良好的线性关系,线性相关系数不小于0.999 7,各元素的检出限在0.64~19.01 ng·L~(-1)之间,加标回收率在89.50%~109.00%之间,相对标准偏差(RSD)在1.17%~4.05%之间,实际样品分析结果显示,食品级壳聚糖中杂质元素的含量较低,其中重金属元素的含量很低,食用安全。该方法能简便、灵敏、准确地测定食品级壳聚糖中的20种杂质元素。
[Abstract]:An inductively coupled plasma mass spectrometry (ICP-MS) method for the direct determination of impurity elements in food grade chitosan was established. Chitosan was dissolved with 3% citric acid and added with low concentration of hydrochloric acid. The ICP-MS method was used to determine the Sn-Sb directly in the presence of ICP-MS. The use of hydrochloric acid can effectively improve the stability of the elements. In particular, Hg and Sn. selective dynamic reaction cell DRCtechnology eliminated the interference of chloride ion and other mass spectra. The matrix matching method was used and ScAY in was added. The mixed solution of Bi internal standard elements compensates for the difference in transport efficiency and the influence of evaporation rate of organic solvent. The standard curve equation of 20 elements has a good linear relationship under the selected working conditions. The linear correlation coefficient was not less than 0.999 7, and the detection limit of each element was between 0.64 ~ 19.01 ng 路L ~ (-1) ng 路L ~ (-1). The recoveries were between 89.50% and 109.00%, and the relative standard deviations (RSDs) were between 1.17% and 4.05%. The content of impurity elements in food grade chitosan is relatively low, and the content of heavy metal elements is very low, which is safe to eat. This method is simple, sensitive and accurate for the determination of 20 impurity elements in food grade chitosan.
【作者单位】：湖南工学院材料与化学工程系;长江师范学院化学化工学院;
【基金】：国家自然科学基金项目(21271187) 重庆市科委前沿与应用基础研究项目(cstc2015jcyjA10053,cstc2015jcyjA10038) 湖南省教育厅重点科研项目(14A035) 湖南省重点学科建设项目(湘教发[2011]76号)资助
【分类号】：O657.63;TS207.3
【正文快照】： 强大的富集作用,食品级壳聚糖中必将存在金属杂质元素,弓|言其含量的高低关系着食品的食用安全,有必要对食品级壳聚糖中的金属杂质元素进行分析。壳聚糖是天然线性多糖甲壳素的衍生物,一般而言,脱壳聚糖不溶于水,能与酸作用发生一NH2质子化反应去55%以上的N-乙酰氨基的甲壳

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