色谱

色谱 ›› 2015, Vol. 33 ›› Issue (5): 541-544.DOI: 10.3724/SP.J.1123.2015.01023

• 技术与应用 • 上一篇    下一篇

高效液相色谱-串联质谱法测定卷烟中的儿茶酚

任志芹1,2, 艾小勇2,4, 黄志强3, 张元2, 王志1, 张峰2   

  1. 1. 河北农业大学理学院, 河北 保定 071001;
    2. 中国检验检疫科学研究院烟草安全与控烟技术中心, 北京 100123;
    3. 湖南检验检疫科学技术研究院, 湖南 长沙 410004;
    4. 华中农业大学植物科技学院, 湖北 武汉 430070
  • 收稿日期:2015-01-21 发布日期:2015-04-23
  • 通讯作者: 王志, 张峰
  • 基金资助:

    质检公益性行业科研专项(201410088,201310134);国家质检总局科技计划项目(2013IK202);国家重大仪器设备开发专项(2012YQ14000806).

Determination of catechol in tobacco by high performance liquid chromatography-tandem mass spectrometry

REN Zhiqin1,2, AI Xiaoyong2,4, HUANG Zhiqiang3, ZHANG Yuan2, WANG Zhi1, ZHANG Feng2   

  1. 1. College of Science, Agricultural University of Hebei, Baoding 071001, China;
    2. Center of Tobacco Safety and Control, Chinese Academy of Inspection and Quarantine, Beijing 100123, China;
    3. Hunan Academy of Inspection and Quarantine, Changsha 410004, China;
    4. College of Plant Science and Technology, Huazhong Agricultural University, Wuhan 430070, China
  • Received:2015-01-21 Published:2015-04-23

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358

被引次数

2

摘要：

建立了一种高效液相色谱-串联质谱(HPLC-MS/MS)测定卷烟中儿茶酚的分析方法。样品经2.5 mol/L硫酸加热回流后用水蒸气蒸馏提取,C18固相萃取柱富集净化后进行HPLC-MS/MS分析,采用甲醇-0.2%(v/v)的甲酸水溶液作为流动相进行梯度洗脱,以电喷雾负离子(ESI-)扫描和多反应监测(MRM)模式对目标物进行定性和定量分析。目标物儿茶酚的含量在0.5~200 μg/kg时与峰面积呈良好的线性关系(r2=0.9989);在样品中添加高、中、低3个水平的标准品,其加标回收率在83.1%~98.6%之间,相对标准偏差(RSD)在1.9%~5.8%之间。应用本方法对6种市售卷烟样品进行了测试,结果从6种市售卷烟中均检出了儿茶酚。该方法操作简单、快速、灵敏度高,适用于卷烟中儿茶酚的检测。

关键词: 儿茶酚, 高效液相色谱-串联质谱法, 固相萃取, 卷烟

Abstract:

An analytical method for the determination of catechol in tobacco by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) has been developed. A Sep-Park-C18 solid phase extraction cartridge was used for the enrichment of the analyte for HPLC-MS/MS analysis. The mobile phase was methanol-0.2% (v/v) formic acid with gradient elution. The sample was analyzed by HPLC-MS/MS in the ESI-scanning mode with multi-reaction monitoring (MRM) for qualitative and quantitative analyses. The linear range of calibration curve was 0.5-200 μg/kg with good correlation coefficients (r2=0.9989). The recoveries of catechol spiked in three levels were in the range of 83.1%-98.6%, with the relative standard deviations of 1.9%-5.8%. This method was initially applied to the research of catechol as a flavor additive in six retail tobacco samples and proved to be accurate, sensitive, convenient and practical. The analyte was found in the six retail tobacco samples, and in some cases, the presence of quite high concentrations of catechol in tobacco should be a matter of concern.

Key words: catechol, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), solid phase extraction (SPE), tobacco

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