色谱

色谱 ›› 2014, Vol. 32 ›› Issue (1): 40-46.DOI: 10.3724/SP.J.1123.2013.08004

• 研究论文 • 上一篇    下一篇

高效液相色谱-紫外/质谱检测法联合测定新鲜烟叶中的25种酚类物质

沈丹红1,2, 路鑫1, 常玉玮1, 张俊杰1, 赵燕妮1, 王瑛2, 许国旺1, 赵春霞1   

  1. 1. 中国科学院大连化学物理研究所, 中国科学院分离分析化学重点实验室, 辽宁 大连 116023;
    2. 南京理工大学化工学院, 江苏 南京 210094
  • 收稿日期:2013-08-01 修回日期:2013-09-16 出版日期:2014-01-08 发布日期:2013-12-26
  • 通讯作者: 赵春霞

Determination of phenolic compounds in fresh tobacco leaves by high performance liquid chromatography-ultraviolet/mass spectrometry

SHEN Danhong1,2, LU Xin1, CHANG Yuwei1, ZHANG Junjie1, ZHAO Yanni1, WANG Ying2, XU Guowang1, ZHAO Chunxia1   

  1. 1. CAS Key Laboratory of Separation Science for Analytical Chemistry, Dalian Institute of Chemical Physics, Chinese Academy of Sciences, Dalian 116023, China;
    2. School of Chemical Engineering, Nanjing University of Science and Technology, Nanjing 210094, China
  • Received:2013-08-01 Revised:2013-09-16 Online:2014-01-08 Published:2013-12-26

PDF

335

被引次数

5

摘要：

建立了烟叶中25种酚类物质的高效液相色谱-紫外/质谱(HPLC-UV/MS)测定方法，其中11种主要酚类物质采用HPLC-UV法进行绝对定量分析，其余采用HPLC-MS法进行半定量分析。方法验证结果表明：11种酚类标准物质在0.90~99.00 mg/L(绿原酸及芸香苷为0.95~380.00 mg/L)范围内呈现很好的线性关系，相关系数为0.9993~0.9999。在22.5~24.8、45.0~49.5、67.5~74.3 mg/L 3个水平的加标回收率为91.0%~112.4%。方法重复性的相对标准偏差(RSD)为1.48%~13.40%，日内日间精密度的RSD为0.35%~15.54%。采用本方法对云南、河南、贵州的成熟期新鲜烟叶样品进行了分析，主要酚类物质总量为贵州>云南>河南，贵州与河南两地间存在显著性差异；芸香苷含量为云南>贵州>河南，且相互间有显著性差异。本方法预处理简单，酚类物质的分析覆盖面广，可用于批量烟叶样品的检测。

关键词: 酚类物质, 高效液相色谱, 烟叶, 质谱, 紫外检测

Abstract:

Twenty-five phenolic compounds in tobacco were analyzed using high performance liquid chromatography-ultraviolet/mass spectrometry (HPLC-UV/MS), including absolute quantification of 11 main phenols by HPLC-UV and relative quantification of other 14 phenols by HPLC-MS. The validation results of this method were satisfactory. Eleven phenol standards showed good linearity with correlation coefficients (r2) of 0.9993-0.9999 over the mass concentration range from 0.90 mg/L to 99.00 mg/L (the range of chlorogenic acid and rutin was from 0.95 mg/L to 380.00 mg/L). The recoveries of the 11 phenol standards were 91.0%-112.4% with the RSDs of 0.33%-8.11% at the three spiked levels of 22.5-24.8, 45.0-49.5 and 67.5-74.3 mg/L. The reproducibility of the method was good with the RSDs of 1.48%-13.40%. In addition, the intra-day and inter-day precisions were also satisfactory with the RSDs of 0.35%-15.54%. Mature fresh tobacco leaves from Yunnan, Henan and Guizhou Provinces, China were analyzed using this method. The results showed that the total amount of main phenols was Guizhou>Yunnan>Henan and there was significant difference between Guizhou and Henan. The amount of rutin was Yunnan>Guizhou>Henan, and there were significant differences among them each other. The method is reproducible with a simple pretreatment covering a wide range of phenols, and can be applied in batch analysis of tobacco leaves.

Key words: high performance liquid chromatography (HPLC), mass spectrometry (MS), phenolic compounds, tobacco leaves, ultraviolet detection

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