一种利用超高效液相色谱-电喷雾离子阱串联质谱(UHPLC-ESI-MS/MS)同时对烟草中的8种糖苷化合物进行定量分析和3种糖苷化合物进行半定量分析的快速有效的方法
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- 英文论文题名：A rapid and efficient method for simultaneous quantitative assessment of eight glycosides and semi-quantitative assessment of three glycosides in tobacco by ultra-high performance liquid chromatography with electrospray ionization tandem mass spectrometry(
- 论文作者：袁月 ; 周容 ; 李东亮 ; 罗成 ; 戴亚
- 年：2016
- 作者机构：四川中烟工业有限责任公司技术研发中心;重庆中烟工业有限责任公司技术研发中心;
- 论文关键词：糖苷化合物 ; 定量分析 ; 超高效液相色谱-电喷雾离子阱串联质谱 ; 烟草
- 英文论文关键词：glycosides ; quantitative analysis ; ultra-high performance liquid chromatography with electrospray ionization tandem mass spectrometry ; tobacco
- 会议召开时间：2016-12-01
- 会议录名称：中国烟草学会2016年度优秀论文汇编——烟草工业主题
- 语种：中文
- 分类号：TS47;O657.63
- 学会代码：ZGYG
- 学会名称：中国烟草学会
- 页数：19
- 文件大小：1531k
- 原文格式：D
摘要
烟草中的糖苷化合物是一类重要的香气前体物,与烟草的质量和吸味特征密切相关。本研究建立了一种基于超高效液相色谱-电喷雾离子阱串联质谱(UHPLC-ESI-MS/MS),能同时对烟草中8种糖苷化合物进行定量分析、3种糖苷化合物进行半定量分析的快速、有效的方法。样品前处理采用了简单的溶剂超声萃取,上机检测则利用电离源的正负极切换和多反应监测模式实现了13分钟的单个样品分析。通过对萃取条件和色谱分离条件的优化,提高了方法的提取效率和灵敏度,8种可定量糖苷化合物的校正曲线相关系数范围从0.9978到0.9999,最低检测限范围从0.06ug/kg到2.18ug/kg,三种浓度的添加回收率范围从71.1%到109.4%,日内精密度和日间精密度分别小于4.1%和5.9%。该方法还成功的用来完成了30个实际烟叶样品中11种糖苷化合物的定量和半定量检测,直观的体现了不同品种、产地、等级烟叶的特征差别,对卷烟产品研发也极具参考价值。
The presence of glycosides in tobacco, as one of the most important aroma precursors, significantly contributes to the quality and flavor characteristics of tobacco products. This study established a rapid and qualitative method for simultaneous quantitative analysis of eight glycosides and semi-quantitative analysis of three glycosides in tobacco, based on ultra-high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry(UHPLC-ESI-MS/MS). The simple solvent extraction for sample preparation combined with chromatographic separation and quantification, using electrospray ionization at both negative and positive modes under multiple-reaction monitoring(MRM) scanning, ensured a single run of 13 minutes. The extraction conditions and equipment parameters were also optimized to improve the selectivity and sensitivity of the method. For the eight quantitative glycosides, the calibration curves showed excellent coefficients of determination(0.9978 ≤ r2 ≤ 0.9999) within the range of tested concentration, and the limit of detection varied from 0.06ug/kg to 2.18ug/kg. Satisfactory values of accuracy(71.1–109.4%) and RSD(intra-day≤4.1%, inter-day≤5.9%) were also achieved. The developed method was successfully applied to determine the investigated 11 glycosides in 30 real tobacco samples, intuitively indicating the difference between tobacco of different species, habitats and classes, providing referential values to the research and development of cigarettes.
The presence of glycosides in tobacco, as one of the most important aroma precursors, significantly contributes to the quality and flavor characteristics of tobacco products. This study established a rapid and qualitative method for simultaneous quantitative analysis of eight glycosides and semi-quantitative analysis of three glycosides in tobacco, based on ultra-high performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry(UHPLC-ESI-MS/MS). The simple solvent extraction for sample preparation combined with chromatographic separation and quantification, using electrospray ionization at both negative and positive modes under multiple-reaction monitoring(MRM) scanning, ensured a single run of 13 minutes. The extraction conditions and equipment parameters were also optimized to improve the selectivity and sensitivity of the method. For the eight quantitative glycosides, the calibration curves showed excellent coefficients of determination(0.9978 ≤ r2 ≤ 0.9999) within the range of tested concentration, and the limit of detection varied from 0.06ug/kg to 2.18ug/kg. Satisfactory values of accuracy(71.1–109.4%) and RSD(intra-day≤4.1%, inter-day≤5.9%) were also achieved. The developed method was successfully applied to determine the investigated 11 glycosides in 30 real tobacco samples, intuitively indicating the difference between tobacco of different species, habitats and classes, providing referential values to the research and development of cigarettes.
引文
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