高效液相色谱-串联质谱法测定卷烟中的儿茶酚

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。

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

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.