[关键词]
[摘要]
目的 建立顶空进样-气质联用(HS-GC-MS)快速分析藏药裂叶独活挥发性成分的方法,分别测定藏药裂叶独活根、茎、叶、花各部位的挥发性成分。方法 采用顶空进样的方式,直接分析裂叶独活根、茎、叶、花的粉末样品。以加热箱温度100℃、样品瓶平衡时间40 min为顶空条件,取样品瓶顶部空间气体1 mL进样入GC-MS系统。建立的GC-MS方法为柱流量1.0 mL/min;分流进样,分流比10:1;进样量1.0 μL;进样口温度为260℃;溶剂延时为3.5 min。程序升温条件:初始温度为50℃(保持2 min),以2℃/min的速度升温至100℃(保持3 min),再以4℃/min的速度升温至220℃(保持3 min)。全扫描模式;扫描范围m/z 50~500。分析结果通过谱库NIST11.L检索,确定裂叶独活中挥发性成分并比较根、茎、叶、花各部分成分的差异。结果 藏药裂叶独活挥发性成分种类主要为醛类、苯类、醇类和烯类物质。根和茎化学成分较为相似,主要成分都有辛醛、己醛和γ-松油烯,但量存在差异。叶和花部位成分较相似,其中邻异丙基苯、异松油烯相对质量分数都在10%以上。与根、茎区别较明显的成分是其中还含有三甲基苯甲醇和(E)-(3,3-二甲基环己亚基)-乙醛。结论 采用HS-GC-MS分析藏药裂叶独活挥发性成分方法可行,操作简便,可以广泛应用于其他中药样品挥发性成分的定性分析。
[Key word]
[Abstract]
Objective To establish a rapid analytical method for volatile components in Tibetan medicine Heracleum millefolium and to determine the volatile components from its roots, stems, leaves, and flower parts, respectively. Methods Headspace sampling incorporation with gas-chromatography-mass spectrum (HS-GC-MS) determination was introduced to analyze the powder directly. Static headspace equilibration was performed at 100℃ for 40 min, and 1 mL of the headspace gas was injected in split mode of 10︰1. The split inlet temperature was 260℃. The carrier gas was He at a constant flow rate of 1.8 mL/min. The column oven temperature was initially set at 50℃ for 2 min, then increased to 100℃ at 2℃/min, held for 6 min, then increased to 300℃ at 10℃/min and held for 2 min. The GC/MS interface temperature was maintained at 280℃. The solvent delay time was 3 min (to bypass the solvent peak). The volatile components were confirmed by NIST11.L database, and volatile organic compounds from roots, stems, leaves, and flower parts were compared. Results The types of compounds in the roots, stems, leaves, and flowers of H. millefolium are mainly aldehyde, benzene, alcohols, and alkene. Octanal, hexanal, and γ-terpinene are the main components in the roots and stems. While o-isopropyltoluene and terpinolene are the main components in the leaves and flowers. Conclusion HS-GC-MS method is easy, simple, and feasible, and can be widely used in other Chinese materia medica samples for analysis of volatile components.
[中图分类号]
[基金项目]
西藏自治区自然科学基金资助项目(2015ZR-14-65);2016年西藏自治区高校青年教师创新支持计划项目(QCZ2016-79);江西省科技支撑计划(20112BBG70021);江西省教育厅项目(GJJ13604)