顶空-气质联用比较不同产地金银花与山银花挥发性成分差异

Comparison of volatile components of Lonicerae japonicae flos and Lonicerae flos from different areas by headspace-gas-mass spectrometry

目的建立快速分析金银花和山银花中挥发性成分的方法,并比较不同产地金银花和山银花的挥发性成分的差异。方法采用顶空-气质(HS-GC-MS)联用技术分析山银花和金银花粉末样品。以加热箱温度150℃、样品瓶平衡时间15 min为顶空条件,取样品瓶顶部空间气体1 mL进样入GC-MS系统进行分析。建立的GC-MS方法为柱流量1.0 mL·min^(-1);分流进样,分流比50∶1;进样口温度为230℃。程序升温条件:初始温度为40℃(保持5 min),以5℃·min^(-1)的速度升温至60℃,再以3℃·min^(-1)的速度升温至100℃,再以4℃·min^(-1)的速度升温至250℃(保持2 min)。全扫描模式;扫描范围m/z 50~500。分析结果通过谱库NIST17.L检索,确定山银花和金银花中挥发性成分并比较其差异,通过聚类分析对不同产区金银花和山银花进行归类。结果共鉴定出86个化合物,其中共有成分8个。金银花中挥发性成分主要为酸类、酯类、酮类、烃类及芳香族化合物,含量上则以酯类、烃类和酮类较高;山银花中主要为醇类和醛类化合物,其酸类、醇类和芳香族化合物含量较高。聚类分析将11批样品分为四类。结论金银花和山银花挥发性成分在数量和含量上均有较大差异。HS-GC-MS分析方法稳定可靠,可用于金银花和山银花中挥发性成分测定,并为金银花和山银花的质量评价提供参考。

Objective To establish a rapid method to analyze the volatile components of Lonicerae japonicae flos and Lonicerae flos,and determine the difference in volatile oils of Lonicerae japonicae flos and Lonicerae flos from different areas.Methods Headspace sampling together with gaschromatography-mass spectrum(HS-GC-MS)was used to analyze the powder directly.Static headspace equilibration was performed at 150℃for 15 min,and 1 mL of the headspace gas was injected in split mode at 50∶1.The split inlet temperature was 230℃.The carrier gas was helium at a constant flow rate of 1.0 mL·min^(-1).The column oven temperature was initially set at 40℃for 5 min,then increased to 60℃at 5℃·min^(-1),then increased to 100℃at 3℃·min^(-1),and further increased to 250℃at 4℃·min^(-1) and held for 2 min.The volatile components were confirmed by NIST17.L database,and the volatile organic compounds of both Lonicerae japonicae flos and Lonicerae flos from different areas were compared.Results A total of 86 compounds were identified,with 8 common volatile components.Acids,esters,ketones,hydrocarbons and aromatic compounds were the main components in Lonicerae japonicae flos,and the content was high in esters,hydrocarbons and ketones.Alcohols and aldehydes were the main components in Lonicerae flos,and the content was higher in acids,alcohols and aromatic compounds.Cluster analysis divided 11 batches of samples into 4 categories.Conclusion The constituents and contents of volatile oils in Lonicerae japonicae flos and Lonicerae flos from different areas are different.HS-GC-MS method is reliable and stable,and can be used to analyze the volatile components in Lonicerae japonicae flos and Lonicerae flos,and provide scientific basis for the quality assessment of Lonicerae japonicae flos and Lonicerae flos.