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.
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