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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 m L进样入GC-MS系统。建立的GC-MS方法为柱流量1.0 m L/min;分流进样,分流比10∶1;进样量1.0μL;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。
OBJECTIVE To establish a rapid method for the analysis of the volatile components in Tibetan medicine leaves by headspace injection-mass spectrometry (HS-GC-MS), and determine the volatile components in the roots, stems, leaves and flowers . Methods Headspace sampling was used to directly analyze the powder samples of root, stem, leaf and flower. The temperature of the heating chamber was 100 ℃ and the equilibrium time of the sample bottle was 40 min. The headspace condition was taken and 1 mL of the space gas was injected into the GC-MS system. The GC-MS method was established with a column flow of 1.0 m L / min; split injection, split ratio of 10: 1; injection volume of 1.0 μL; inlet temperature of 260 ° C .; solvent delay of 3.5 min. Temperature programmed conditions: initial temperature 50 ° C (hold for 2 min), ramp to 100 ° C at 2 ° C / min (hold for 3 min) and ramp to 220 ° C at 4 ° C / min (hold for 3 min). Full scan mode; scanning range m / z 50 ~ 500. The results of the analysis were searched through the NIST11.L library to determine the volatile components of the independent living leaves and to compare the differences in the components of the roots, stems, leaves and flowers. Results The main components of the volatile components in the leaves of Tibetan medicine were aldehydes, benzene, alcohols and alkenes. The chemical composition of roots and stems are similar, the main components are octanal, hexanal and γ-terpinene, but there are differences in quantity. The components of leaves and flowers were similar, with the relative mass fraction of o-isopropylbenzene and terpinolene being more than 10%. The obvious difference between root and stem is that it also contains trimethylbenzyl alcohol and (E) - (3,3-dimethylcyclohexylidene) -acetaldehyde. Conclusion The HS-GC-MS method is simple and easy to operate and can be applied to the qualitative analysis of volatile components in Tibetan medicine samples.