| 江波,黄建华.应用ICP-MS/MS准确测定紫苏籽油中的重金属元素[J].中国粮油学报,2019,34(1):125- |
| 应用ICP-MS/MS准确测定紫苏籽油中的重金属元素 |
| Accurate determination of heavy metal elements in Perilla seed oil using ICP-MS/MS |
| 投稿时间：2018-04-03 修订日期：2018-06-02 |
| DOI： |
| 中文关键词: 紫苏籽油 电感耦合等离子体串联质谱 重金属元素 MS/MS模式 质量转移 |
| 英文关键词:Perilla seed oil inductively coupled plasma tandem mass spectrometry heavy metal elements MS/MS mode mass shift |
| 基金项目:国家自然科学基金项目 |
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| 摘要点击次数: 402 |
| 全文下载次数: 261 |
| 中文摘要: |
| 紫苏籽油中重金属元素的准确测定仍然是食品安全的重要分析任务。本文基于电感耦合等离子体串联质谱(ICP-MS/MS)建立了快速准确测定紫苏籽油中Cr、As、Cd、Hg、Pb的分析方法。对于测定过程中Cr和As所面临的严重干扰,在MS/MS模式下,采用O<sub>2</sub>为反应气,通过质量转移反应将Cr<sub>+</sub>和As<sub>+</sub>转移为CrO<sub>+</sub>和AsO<sub>+</sub>实现无干扰测定,而对于Cd、Hg、Pb测定过程中存在的干扰轻微可以忽略不计,仍然可以在MS/MS模式下使用无气方式使待测离子运行的质谱通道更加畅通,提高待测离子的传输效率。采用建立的方法,所有元素在0-50 μg/L的范围内具有良好的线性关系(R<sub>2</sub>≥0.9997),应用三水平加标回收实验评估了方法的准确性,各元素的加标回收率在92.5%-108.0%之间,相对标准偏差(RSD)≤4.1%。Cr、As、Cd、Hg、Pb的检出限分别为3.26、1.91、0.84、2.25、0.89 ng/L,方法已应用于紫苏籽油中重金属元素的测定。实际样品的ICP-MS/MS分析结果表明,紫苏籽油中Cr、As、Cd、Hg、Pb的含量极低,不会对人体构成潜在危害。 |
| 英文摘要: |
| Accurately determination of heavy metal elements in Perilla seed oil is still a critical analytical task for food safety estimation. In this paper, a rapid and accurate analytical method for the absolutely determination of Ni, As, Cd, Hg, and Pb in Perilla seed oil based on inductively coupled plasma tandem mass spectrometry (ICP-MS/MS) was established. In the MS/MS mode, O2 was used as the reaction gas to transform Cr+ and As+ to CrO+ and AsO+, which can realize interference-free measurement by mass shift method to overcome the serious interference of Cr and As. The slight interference to Cd, Hg, and Pb could be negligible. Even in the MS/MS mode, the no gas mode can still be used to make the ion operation channel more open and improve the transmission efficiency of the analytes. The developed method exhibited good linear relationship for analytes in the 0-50 μg/L range (R2≥0.9997). The accuracy of method was evaluated by spike experiments, their recoveries range from 92.5% to 108.0%for analytes. Relative standard deviation (RSD) was lower than 4.1%. The detection limits of element Cr, As, Cd, Hg, and Pb were 3.26, 1.91, 0.84, 2.25, and 0.89 ng/L, respectively. The method has been successfully applied to the determination of heavy metal elements in Perilla seed oil. The results of ICP-MS/MS analysis of real samples showed that the contents of Cr, As, Cd, Hg and Pb in Perilla seed oil were very low, and would not pose potential harm to human body. |
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