高效液相色谱-电感耦合等离子体质谱法测定紫菜中的碘形态  

Determination of iodine species in seaweed samples using high performance liquid chromatography-inductively coupled plasma mass spectrometry

作　　者：刘崴[1] 曹蔚然 胡俊栋[1] 杨红霞[1] 

机构地区：[1]国家地质实验测试中心,北京100037 [2]中国地质大学,武汉430074

出　　处：《分析试验室》2017年第9期1028-1031,共4页Chinese Journal of Analysis Laboratory

基　　金：国家自然科学基金项目(41301565);中国地质科学院基本科研业务费项目(YYWF201620)资助

摘　　要：建立了高效液相色谱-电感耦合等离子体质谱(HPLC-ICP-MS)联用技术测定紫菜中IO_3^-,I^-,MIT和DIT的方法。采用离子交换色谱柱AS7分离4种碘形态,以175 mmol/L NH_4NO_3和4%(V/V)甲醇为流动相,在梯度洗脱的条件下可实现4种碘形态的完全分离。在此条件下,IO_3^-,I^-,MIT和DIT的方法检出限(以碘计)分别为0.09,0.34,0.09,0.33μg/L,可满足紫菜中碘形态的测定要求。对紫菜样品前处理方法进行了优化比较,最终确定40℃超声提取2次,每次超声2 h为紫菜样品前处理方法,方法可保持样品处理过程中各碘形态的稳定。利用建立的方法并结合体积排阻色谱对紫菜标准物质GSB-14中的碘形态进行分析,发现其主要以I^-和一种未知碘形态存在。A quantitative method of IO3^-,I^-,MIT and DIT in seaweed using high performance liquid chromatography coupled with inductively coupled plasma mass spectrometry was established. AS7 anion exchange column was selected as a separation column and the mobile phase was 175 mmol/L ammonium nitrate plus 4 %（ V/V） methanol with gradient eluting. The detection limits for IO3^-,I^-,MIT and DIT were 0. 09,0. 34,0. 09 μg/L and 0. 33 μg/L,respectively. The sample preparation methods were optimized and the ultrasound method with 2 h at 40 ℃ was chosen finally. The recoveries of IO3^-,I^-,MIT and DIT were between 80 % and 120 %. Iodine speciation of a seaweed standard（ GSB-14） was analyzed using this method and size exclusion chromatography（ SEC）. I--and an unknown iodine specie were detected in the GSB-14.

关 键 词：碘 形态分析 紫菜 高效液相色谱-电感耦合等离子体质谱 

分 类 号：TS201.6[轻工技术与工程—食品科学]