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高效液相色谱-电感耦合等离子体质谱法测定土壤中不同形态的无机碘
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胡梦娜,周启星,陈翠红,刘维涛 南开大学环境科学与工程学院环境污染过程与基准教育部重点实验室天津市城市环境污染诊断与修复工程技术中心 
基金项目:国家自然科学基金面上项目(21677080);高等学校学科创新引智计划(111计划)资助”(T2017002);中央高校基本科研业务费专项资金;国家自然科学基金委-山东省政府联合基金重点项目(U1806216)
中文摘要:建立了一种有效分离检测土壤中不同形态无机碘(碘离子和碘酸根离子)的高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)。采用4 mmol/L四丁基氢氧化铵(TBAH)溶液为提取剂进行超声提取,经离心分层,过Na柱和022 μm滤膜后进行分析,以50 mmol/L碳酸铵溶液(pH 9.8,以25%氨水调节)为流动相,采用AS16阴离子分析柱进行HPLC-ICP-MS测定。结果表明,在优化实验条件下,两种无机碘形态(I-和IO-3)在10~500 μg/L范围内线性关系良好,相关系数(r2)均大于0.999,检出限分别为0.05、0.1 μg/L,定量下限分别为2、5 μg/L。该方法用于土壤环境中无机碘的测定,其加标回收率为83.8%~108%,相对标准偏差(RSD)为0.5%~3.0%,优于振荡提取法。该方法快速、高效、重现性好、灵敏度高,适用于土壤环境中不同形态无机碘的测定。
中文关键词:高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS);土壤环境;无机碘  形态
 
Determination of Different Inorganic Iodine Species in Soils by High Performance Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry
Abstract:A method was established for the separation and determination of different inorganic iodine species(iodide and iodate ions) in soils by high performance liquid chromatography and inductively coupled plasma-mass spectrometry(HPLC-ICP-MS).The sample was ultrasonically extracted with 4 mmol/L tetrabutylammonium hydroxide(TBAH) solution.After centrifugation,the sample was purified with Na column and 022 μm hybrid filter membrane.The determination was performed by HPLC-ICP-MS combined with a Dionex IonPac AS16 anion exchange column using 50 mmol/L ammonium carbonate(pH 9.8) as mobile phase.Results indicated that the linear ranges for two inorganic iodine species(I- and IO-3) ranged from 10 μg/L to 500 μg/L with correlation coefficients(r2) greater than 0.999.The limits of detection for the two iodine species were 0.05 μg/L and 0.1 μg/L,and the limits of quantitation were 2 μg/L and 5 μg/L,respectively.The method was applied in the determination of two inorganic iodine species in soils,with spiked recoveries of 83.8%-108%and relative standard deviations(RSD) of 0.5%-3.0%,which were better than those obtained by the oscillation extraction.With the advantages of rapidness,high efficiency,good reproducibility and high sensitivity,the method is suitable for the determination of different inorganic iodine species in soils.
Key Words:high performance liquid chromatography-inductively coupled plasma-mass spectrometry(HPLC-ICP-MS)  soil  inorganic iodine  species
引用本文:胡梦娜,周启星,陈翠红,刘维涛.高效液相色谱-电感耦合等离子体质谱法测定土壤中不同形态的无机碘[J].分析测试学报,2019,38(11):1389-1392.
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