3种嘌呤生物碱在卷烟烟气中转移行为研究
Study on the transfer behavior of three purine alkaloids in cigarette smoke
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摘要: 【目的】 探究3种嘌呤生物碱的裂解规律及其在卷烟烟气中的转移行为。【方法】 通过热裂解-气相色谱/质谱联用(Py-GC/MS)技术研究可可碱、茶碱、咖啡因的热裂解行为,建立适用于卷烟主流烟气中3种生物碱的超高液相色谱-高分辨质谱联用(UPLC-HRMS)技术的半定量分析方法,优化前处理条件并测定生物碱在卷烟烟气中的转移率。【结果】 在300 ℃和600 ℃的热解温度范围内,3种生物碱均以原型转移为主,当裂解温度升至900 ℃时,其裂解程度显著增强,含量明显下降,且在热裂解过程中没有多环芳烃类物质生成;当萃取溶剂为NaOH溶液(pH值为11.9),萃取方式为回流萃取,萃取时间为4.0 h,测试方法为UPLC-HRMS,3种生物碱的加标回收率最高,满足半定量分析技术要求;可可碱、茶碱、咖啡因在卷烟主流烟气中的转移率分别为0.21%、0.74%、0.10%,其中茶碱的转移率最高。【结论】 基于3种嘌呤生物碱的高温转移规律构建的烟草复杂基质中痕量生物碱的分析技术体系,可为烟草制品的质量控制与健康风险评估,以及高沸点香料成分的烟气转移行为研究提供参考。
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关键词:
- 卷烟 /
- 生物碱 /
- 热裂解 /
- 超高液相色谱-高分辨质谱联用技术 /
- 转移行为
Abstract: 【Objective】 To investigate the pyrolysis characteristics of three purine alkaloids and their transfer behaviors in cigarette smoke. 【Methods】 The pyrolysis behaviors of theobromine, theophylline, and caffeine were investigated by pyrolysis-gas chromatography/mass spectrometry (Py-GC/MS) hyphenation. A semi-quantitative analytical method using ultra-high performance liquid chromatography-high resolution mass spectrometry (UPLC-HRMS) was established for the semi-quantitative determination of the three alkaloids in mainstream cigarette smoke, and the pretreatment conditions were optimized to determine the transfer rates of the alkaloids in mainstream cigarette smoke. 【Results】 In the pyrolysis temperature range of 300 ℃ and 600 ℃, the three alkaloids were predominantly transferred in their original form; however, when the pyrolysis temperature increased to 900 ℃, their pyrolysis extent was significantly enhanced and their contents decreased markedly, and no polycyclic aromatic hydrocarbons (PAHs) were generated during pyrolysis. The highest spiked recoveries of the three alkaloids were obtained under the following optimized conditions: extraction solvent: NaOH solution (pH value 11.9), extraction method: reflux extraction, extraction time: 4.0 h, and detection method: UPLC-HRMS, which met the technical requirements of semi-quantitative analysis. The transfer rates of theobromine, theophylline, and caffeine in mainstream cigarette smoke were 0.21%, 0.74%, and 0.10%, respectively, with theophylline having the highest transfer rate. 【Conclusion】 Based on the high-temperature transfer characteristics of the three purine alkaloids, an analytical technology system for trace alkaloids in complex tobacco matrices was constructed. This system can provide a reference for the quality control of tobacco products, their health risk assessment, as well as the study on the smoke transfer behaviors of high-boiling-point flavor components. -
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