CAJ | 학술논문

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。
건립료일충고효액상색보-천련질보（ HPLC-MS／MS）측정권연중인다분적분석방법。양품경2.5 mol／L 류산가열회류후용수증기증류제취，C18고상췌취주부집정화후진행 HPLC-MS／MS 분석，채용갑순-0.2％（ v／v）적갑산수용액작위류동상진행제도세탈，이전분무부리자（ ESI-）소묘화다반응감측（ MRM）모식대목표물진행정성화정량분석。목표물인다분적함량재0.5~200μg／kg 시여봉면적정량호적선성관계（ r2=0.9989）；재양품중첨가고、중、저3개수평적표준품，기가표회수솔재83.1％~98.6％지간，상대표준편차（ RSD）재1.9％~5.8％지간。응용본방법대6충시수권연양품진행료측시，결과종6충시수권연중균검출료인다분。해방법조작간단、쾌속、령민도고，괄용우권연중인다분적검측。
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.