基于全二维气相色谱-四极杆飞行时间质谱法比较顶空-固相微萃取法和同时蒸馏法对砂仁中挥发性成分的提取效果

Comparison of Extraction Effect of Headspace-Solid Phase Microextraction and Simultaneous Distillation on Volatile Components in Amomum Villosum Based on Comprehensive Two-Dimensional Gas Chromatography-Quadrupole Time-of-Flight Mass Spectrometry

基于全二维气相色谱-四极杆飞行时间质谱法(GC×GC-QTOFMS)比较顶空-固相微萃取法(HS-SPME)和同时蒸馏法对砂仁中挥发性成分的提取效果。将样品四分法缩分、过筛后,分别用同时蒸馏法和HS-SPME(平衡温度设置为50℃,平衡、萃取时间分别设置为5,50 min)提取,用GC×GC-QTOFMS测定,用SIMCA 14.1和SPSS17.0软件进行主成分-判别分析(PCA-DA)和正交偏最小二乘法-判别分析(OPLS-DA),以确认两种方法的产地和批次鉴别能力以及区分两种方法的差异性成分。结果显示:HS-SPME和同时蒸馏法检出成分分别有162,178种,HS-SPME检出萜类化合物和烯烃类化合物含量明显高于同时蒸馏法的。检出的相对含量大于1.00%(以面积归一化法计算)的成分基本一致。PCA-DA结果显示,HS-SPME的产地和批次鉴别能力更强。OPLS-DA结果显示,可筛选出22种差异性成分用于区分两种方法,其中α-松油醇、α-没药醇和α-香柠檬醇为极显著差异性成分。

Based on comprehensive two-dimensional gas chromatography-quadrupole time-of-flight mass spectrometry(GC×GC-QTOFMS),the extraction effect of headspace-solid phase microextraction(HS-SPME)and simultaneous distillation on volatile components in Amomum villosum was compared.After quartering and sieving,the sample was extracted by simultaneous distillation and by HS-SPME with equilibrium temperature of 50℃under time of equilibriun and extraction of 5,50 min,respectively,then analyzed by GC×GC-QTOFMS.Softwares of SIMCA 14.1 and SPSS17.0 were used for PCA-DA and OPLS-DA,to confirm the ability of the above 2 methods to identify origin and batch,as well as distinguish their differential components.As found by results,162,178 kinds of volatile components were detected by HS-SPME and simultaneous distillation,respectively.The terpenoids and alkenes detected by HS-SPME were significantly higher than those detected by simultaneous distillation.The components with relative content greater than 1.00%(calculated by the area normalization method)were basically the same.In the PCA-DA analysis,HS-SPME had stronger ability to identify the origin and batch.In the OPLS-DA analysis,22 differential components could be screened to distinguish between the 2 methods,among whichα-terpineol,α-bisabolol andα-bergamot were extremely significant differential components.