咳喘浸手浴足Ⅰ号挥发性成分的顶空-气相色谱-质谱分析

Headspace Sampling-Gas Chromatography-Mass Spectrometry Analysis of Volatile Components of Kechuan Jinshou Yuzu PowderⅠ

目的:分析咳喘浸手浴足Ⅰ号挥发性成分,为该中药复方制剂的进一步研究提供参考。方法:应用顶空静态加热萃取技术提取咳喘浸手浴足Ⅰ号挥发性成分,采用顶空-气相色谱-质谱(HS-GC-MS)联用技术分析,使用Agilent DB-5MS毛细管色谱柱(0.25μm×0.25 mm×30 m)分离,程序升温条件为初始温度40℃,保持3 min,以4℃/min升至120℃,保持5 min,以8℃/min升至160℃,保持5 min;载气为高纯氦气(纯度≥99.999%),载气流量1.0 m L/min;分流比100∶1,进样口温度200℃,进样量1μL;质谱条件:电离方式EI,轰击电压70 eV,正离子模式,离子源温度230℃。结果:从10批样品得到的HS-GC-MS图谱中共识别17个共有峰,结合文献识别为2,3,5,6-四甲基吡嗪(No.12,含量3.34%)、D-柠檬烯(No.8,含量16.26%)和α-蒎烯(No.3,含量6.94%)等相关物质。结论:本研究揭示了咳喘浸手浴足Ⅰ号挥发性成分的组成情况,其中可能主要有效成分为2,3,5,6-四甲基吡嗪、D-柠檬烯和α-蒎烯,同时含有月桂烯、β-蒎烯、蒈烯等萜类透皮吸收促渗剂。

Objective:To analyze the volatile components of Kechuan Jinshou Yuzu powderⅠ,so as to provide reference for further study of traditional Chinese medicine compound preparation.Methods:Volatile components of Kechuan Jinshou Yuzu powder I were extracted by using headspace static heating extraction technology.Headspace sampling-gas chromatography-mass spectrometry(HS-GC-MS)technology was used for analysis.Agilent DB-5 MS capillary column(0.25μm×0.25 mm×30 m)was used for separation.The programmed temperature was set as the initial temperature of 40℃,which was maintained for 3 min,then increased to 120℃at 4℃/min,maintained for 5 min,and increased to 160℃at 8℃/min,maintained for 5 min.The carrier gas was high-purity helium(purity≥99.999%),with the carrier gas flow rate of 1.0 m L/min.The splitting ratio was 100∶1,inlet temperature was 200℃and injection volume was 1μL.Mass spectrometry conditions:ionization mode EI,bombardment voltage 70 eV,positive ion mode,ion source temperature 230℃.Results:The HS-GC-MS map obtained from 10 samples identified 17 common peaks,including 2,3,5,6-tetraminepyrazine(No.12,3.34%),D-limonene(No.8,16.26%),α-pinene(No.3,6.94%)and other related substances.Conclusion:This study reveals the composition of volatile components of Kechuan Jinshou Yuzu powderⅠ,among which the main effective components may be 2,3,5,6-tetramethylpyrazine,D-limonene andα-pinene,as well as transdermal absorption enhancers including myrcene,β-pinene and carene.