色谱 ›› 2016, Vol. 34 ›› Issue (10): 986-988.DOI: 10.3724/SP.J.1123.2016.06015

• 特别策划:离子态化合物色谱分析专栏 • 上一篇    下一篇

离子色谱-串联质谱法检测茶叶中的高氯酸盐

刘小芳1, 方从容2, 刘慧3, 李仁勇3, 阎超1   

  1. 1. 上海交通大学药学院, 上海 200240;
    2. 国家食品安全风险评估中心, 北京 100021;
    3. 赛默飞世尔科技(中国)有限公司, 上海 201206
  • 收稿日期:2016-06-12 出版日期:2016-10-08 发布日期:2013-04-03
  • 通讯作者: 阎超
  • 基金资助:

    国家自然科学基金项目(21175092);上海市科委科研计划项目(15142200200);上海市教育委员会科研创新项目(14YZ170);中国博士后科学基金资助项目(2015M581628).

Determination of perchlorates in tea by ion chromatography- tandem mass spectrometry

LIU Xiaofang1, FANG Congrong2, LIU Hui3, LI Renyong3, YAN Chao1   

  1. 1. School of Pharmacy, Shanghai Jiao Tong University, Shanghai 200240, China;
    2. China National Center for Food Safety Risk Assessment, Beijing 100021, China;
    3. ThermoFisher Scientific (China) Corporation, Shanghai 201206, China
  • Received:2016-06-12 Online:2016-10-08 Published:2013-04-03
  • Supported by:

    National Natural Science Foundation of China (No. 21175092); Research and Development Program of Shanghai Municipal Science and Technology Commission (No. 15142200200); Innovation Program of Shanghai Municipal Education Commission (No. 14YZ170); China Postdoctoral Science Foundation Funded Project (No. 2015M581628).

摘要:

建立了离子色谱-串联质谱检测茶叶中高氯酸盐的分析方法。选用高容量、强亲水性的IonPac AS20阴离子交换柱(2 mm)进行分离,以淋洗液自动发生器在线产生的70 mmol/L氢氧化钾为淋洗液等浓度淋洗,TSQ Quantiva三重四极杆质谱仪作检测器,采用电喷雾电离源负离子(ESI-)模式、多反应监测(MRM)模式进行分析,内标法定量。结果表明,高氯酸盐在0.02~10.0 μg/L范围内线性关系良好,相关系数(r)为0.9991,定量限为2 μg/kg。运用该方法测定5种茶叶中的高氯酸盐,加标回收率为87.3%~112.2%。该方法具有操作简单、专属性强、灵敏度高等优点,可满足茶叶中高氯酸盐的检测要求。

关键词: 茶叶, 高氯酸盐, 离子色谱-串联质谱

Abstract:

A rapid ion chromatography-tandem mass spectrometry(IC-MS/MS) method was developed for the determination of perchlorates in tea. The chromatographic analysis was performed on Dionex 5000+, using high capacity and hydroxide selective column IonPac AS20 (2 mm). Perchlorates were separated by isocratic elution with 70 mmol/L KOH eluent generated from on-line eluent generation cartridge. TSQ QuantivaTM, as a detector, scanned samples and monitored multi ion pairs simultaneously for confirmation and quantification, in the mode of negative ESI and multiple reaction monitoring (MRM). The results displayed good linearity in the range of 0.02-10.0 μg/L, with correlation coefficient (r) of 0.9991. The relative standard deviations (RSDs) were 2.67% (n=5). The limits of quantification of the method were 2 μg/kg. The average recoveries of perchlorates in the five kinds of tea ranged from 87.3% to 112.2%. The results showed that the method is fast, simple, selective, sensitive and suitable for the determination of perchlorates in various complex matrix samples such as tea.

Key words: ion chromatography-tandem mass spectrometry (IC-MS/MS), perchlorates, tea

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