高效液相色谱-串联质谱法测定卷烟中的儿茶酚  

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

作　　者：任志芹 艾小勇[2,3] 黄志强 张元[2] 王志[1] 张峰[2] 

机构地区：[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]华中农业大学植物科技学院,湖北武汉430070 [4]湖南检验检疫科学技术研究院,湖南长沙410004

出　　处：《色谱》2015年第5期541-544,共4页Chinese Journal of Chromatography

基　　金：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)

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0.5~200μg／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。An analytical method for the determination of catechol in tobacco by high perform-ance 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-reac-tion monitoring（ MRM）for qualitative and quantitative analyses. The linear range of calibration curve was 0. 5-200 μg/kg with good correlation coefficients（ r 2=0. 998 9 ）. 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 fla-vor 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 pres-ence of quite high concentrations of catechol in tobacco should be a matter of concern.

关 键 词：固相萃取 高效液相色谱-串联质谱法 儿茶酚 卷烟 

分 类 号：O658[理学—分析化学]