微波辅助提取-气相色谱-质谱联用快速分析花椒挥发油

Analysis of Volatile Oil Composition of Pricklyash Peel(Zanthoxylum bungeanum)by Microwave Assisted Steam Distillation Coupled with Gas Chromatography-Mass Spectrometry

建立微波辅助提取-气相色谱-质谱联用快速分析花椒挥发油的方法。采用微波辅助提取-水蒸气蒸馏法(MAE-SD)提取挥发油,正交试验设计优化微波辅助提取条件,气相色谱-质谱联用分析挥发油的化学成分和理化性质,同时将微波辅助提取与传统水蒸气蒸馏法进行比较。结果表明:MAE-SD的最佳工艺为微波功率400W、加水量15mL/g、浸泡30min,提取20min;经GC-MS分析,分离得到137种成分,质谱鉴定相似度在90%以上的化合物59种;根据峰面积归一法,相对含量较高的成分有桧萜(3.72%)、β-月桂烯(8.34%)、枞萜(15.15%)、松油烯(3.65%)、桉树脑(6.25%)、α-蒎烯(4.95%)、β-芳樟醇(3.05%)、4-萜品醇(10.48%)、松油醇(3.55%)、α-松油醇酯(4.09%);与水蒸气蒸馏法相比,挥发油的成分种类和理化性质接近,但相对含量存在一定差异。MAE-SD可快速高效提取挥发油类成分,联合GC-MS可对挥发油进行快速分析。

In the extraction of volatile oil from pricklyash peel by microwave-assisted steam distillation（MASD）,main extraction parameters were optimized by orthogonal assay design based on extraction efficiency with the purpose of developing a sample preparation method for rapid analysis of volatile oil composition of pricklyash peel by gas chromatography-mass spectrometry（GC-MS）.The effects of MASD and single steam distillation on the extraction efficiency,physicochemical properties and chemical composition of volatile oil from pricklyash peel were compared.The optimal MASD parameters were determined as follows：microwave power 400 W,extraction time 20 min,and the amount of water addition 15 mL/g.Totally,137 compounds were separated in the GC-MS analysis of volatile oil extracted by MASD,and 59 of them had higher than 90%mass spectral similarities,including the dominant compounds sabinene（3.72%）,beta-myrcene（8.34%）,sylvestren（15.15%）,terpinene（3.65%）,cineole（6.25%）,alpha-pinene（4.95%）,beta.-linalool（3.05%）,4-carvomenthenol（10.48%）,alpha-terpieol（3.55%） and alpha-terpineol acetate（4.09%）,which were quantitatively determined by peak area normalization method.Volatile oils extracted by both methods had similar compound composition and physicochemical properties but differed in the relative contents of their common components.In summary,an efficient and effective extraction of volatile oil can be achieved by using MASD.Volatile oil composition can be rapidly analyzed by MASD coupled with GC-MS.