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在线LC-GC/MS联用技术开发及其在电子烟液香味成分分析中的应用
Development and application of on-line coupled Liquid Chromatography–Gas Chromatography/Mass Spectrometry for the analysis of flavor constituents in e-liquid
【Author】 GAO Yihan;ZHENG Saijing;LIU Baizhan;Shanghai Tobacco Group Co.Ltd.,Technology R&D Center;
【机构】 上海烟草集团有限责任公司技术研发中心;
【摘要】 本文开发了一种新颖的液相色谱-气相色谱/质谱联用(LC-GC/MS)分析电子烟液香味成分方法,首次运用双三通气路,开发了无阀压力切换的LC-GC接口技术,利用柱反吹,解决了溶剂蒸汽进入质谱的问题,有效降低高沸点物质对GC/MS的污染,且更换色谱柱时质谱无须放真空,并可充分利用溶剂效应,减少低沸点香味成分损失。采用该技术对不同口味的电子烟液进行分析,利用硅胶液相色谱柱去除甘油、丙二醇和烟碱,将香味物质段转入GC/MS分析。通过异丙醇萃取LC-GC/MS与溶剂萃取-GC/MS方法比较,结果表明:对于GC/MS分析,正己烷对极性香味物质萃取不完全,异丙醇无法避免甘油、丙二醇的干扰;异丙醇萃取LC-GC/MS方法既可彻底去除丙二醇、甘油和烟碱对香味成分的干扰,又能保证极性香味物质检测。此方法灵敏度高,重复性好,溶剂用量少,前处理简单,仪器全自动运行,适于大批量样品检测。
【Abstract】 A novel fully automated on-line coupled Liquid Chromatography–Gas Chromatography/Mass Spectrometry(LC-GC/MS) method was developed to analyze of electronic cigarettes e-liquid. Two Y splits were introduced to the pressure-free switch LC-GC interface, which prevent the inhaling solvent into the mass spectrometry detector, and the column could be changed easily without venting; The interface described above allow the high boiling point components to be expelled via the blackflush gas, the influence of solvent on the mass spectrometry detector could be avoided completely; The solvent trapping effects can reduce the loss of volatile components. The established online LC-GC/MS method was used to analyze flavor constituents in commercial brand electronic cigarettes liquid. By using silica gel column and employing liquid chromatography technique, glycerol and propylene glycol were removed while the analyte would be transferred into the GC/MS. Compared with the solvent extraction-GC/MS analysis, the isopropanol extraction-LC-GC/MS method can avoid the influence of glycerol and propylene glycol, and the polarity components in e-liquid could be detected. The results showed that the method has the advantages of simple preparation, less solvent consumption, good reproducibility and sensitivity, suitable for multitudinous samples of routine analysis.
【Key words】 E-cigarette; E-liquid; LC-GC/MS; Flavor constituents;
- 【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
- 【会议时间】2016-12
- 【分类号】TS411