超声辅助氨水提取-ICP-MS法测定矿物质预混料中总碘
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摘要
试验建立了电感耦合等离子体质谱(ICP-MS)测定矿物质预混料中碘元素的方法,优化了氨水浓度及超声时间等因素对提取的影响,并探讨了提取液的稳定性。结果表明,在超声40 min条件下, 20%氨水溶液可较好地提取矿物质预混料中的总碘,碘可稳定存在于提取液48 h;以103Rh作为在线内标,采用4 mL/min氦气碰撞池模式的ICP-MS法测定碘含量,碘的线性范围为0～200μg/L,线性相关系数R为0.999 8,方法检出限为0.015 mg/kg。对预混料样品加入低、中、高三个梯度标物测定,回收率在95%～105%之间,重复性RSD为2.6%,再现性RSD为1.4%, n=7。该方法准确、便捷、回收率良好,适用于不同矿物质预混料中总碘含量的测定。
A method for the determination of iodine in mineral premix by inductively coupled plasma mass spectrometry(ICP-MS) was established. The effects of ammonia concentration and ultrasonic time on the extraction were optimized, and the stability of the extract was discussed. The results showed that the total iodine in mineral premix could be extracted by 20% ammonia solution under the condition of ultrasonic for 40 min, and iodine could stably exist in the extract for 48 h. The iodine content was determined by 4 mL/min helium collision cell mode ICP-MS with 103 Rh as the on-line internal standard. The linear range of iodine was 0-200 μg/L, the linear correlation coefficient R was 0.999 8, and the detection limit was 0.015 mg/kg. The recoveries were 95%-105% when three gradient standards were added to the premix sample. The reproducibility of RSD was 2.6%, and the reproducibility of RSD was 1.4%, n=7. The method was accurate, convenient and good in repeatability, reproducibility and recovery rate, and it was suitable for the determination of total iodine content in different mineral premix.
A method for the determination of iodine in mineral premix by inductively coupled plasma mass spectrometry(ICP-MS) was established. The effects of ammonia concentration and ultrasonic time on the extraction were optimized, and the stability of the extract was discussed. The results showed that the total iodine in mineral premix could be extracted by 20% ammonia solution under the condition of ultrasonic for 40 min, and iodine could stably exist in the extract for 48 h. The iodine content was determined by 4 mL/min helium collision cell mode ICP-MS with 103 Rh as the on-line internal standard. The linear range of iodine was 0-200 μg/L, the linear correlation coefficient R was 0.999 8, and the detection limit was 0.015 mg/kg. The recoveries were 95%-105% when three gradient standards were added to the premix sample. The reproducibility of RSD was 2.6%, and the reproducibility of RSD was 1.4%, n=7. The method was accurate, convenient and good in repeatability, reproducibility and recovery rate, and it was suitable for the determination of total iodine content in different mineral premix.
引文
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[14]钟志光,何颖贤,李政军,等.智能稀释DUO-ICP-AES测定密封不锈钢食品容器中铅、镉、铬、镍溶出量[J].润滑与密封, 2009(10):87-91.
[2]吴勣. ICP-MS测定大气颗粒物中的碘物种[J].上海师范大学学报(自然科学版), 2013(2):173-177.
[3]张亚平,张淑琼,黄三发. ICP-MS分析技术及其在微量元素碘测定中的应用[J].海峡预防医学杂志, 2008(2):17-20.
[4]李姗,何霜,李吉龙,等. KOH快速消解/ICP-MS测定婴幼儿乳粉中总碘含量[J].分析测试学报, 2016(7):864-868.
[5]王瑞敏.电感耦合等离子体质谱法(ICP-MS)测定紫菜中微量碘[J].饮料工业, 2010(12):20-22.
[6]莫曦明,梁旭霞,陈砚朦,等.电感耦合等离子体质谱法(ICP-MS)测定饮用水中碘元素[J].中国卫生检验杂志,2006, 16(10):1179-1180.
[7]彭寨玉,莫曦明,杨挺立,等.电感耦合等离子体质谱法(ICP-MS)测定尿中碘[J].中国卫生检验杂志, 2007,17(11):1946-1947.
[8]左书梅. ICP-MS测定生活饮用水中碘含量[J].医学动物防制, 2014(12):1374-1375, 1390.
[9]巩海娟,李东雷. ICP-MS检测水中碘的方法研究[J].吉林地质, 2015(1):123-125.
[10]王旭日.电感耦合等离子体质谱法测定水体中溴和碘量[J].理化检验(化学分册), 2015(8):1187-1190.
[11]赵秋香,汪模辉,刘赛红.电感耦合等离子体质谱仪同时测定地下水中的溴和碘[J].光谱实验室, 2009(6):1519-1522.
[12]HALDIMANNM,EASTGATEA,ZIMMERLIB.Improved measurement of iodine in food samples using inductively coupled plasma isotope dilution mass spectrometry[J].Analyst, 2000, 125:1977-1982.
[13]张明仁.电感耦合等离子体质谱法测定茶叶中微量碘[J].当代化工, 2010, 39(2):222-223.
[14]钟志光,何颖贤,李政军,等.智能稀释DUO-ICP-AES测定密封不锈钢食品容器中铅、镉、铬、镍溶出量[J].润滑与密封, 2009(10):87-91.