多次顶空固相微萃取在大曲挥发性化合物定量中的应用

Application of multiple headspace solid phase microextraction in quantification of volatile compounds in daqu

应用顶空固相微萃取(headspace solid-phase microextraction,HS-SPME)结合气相色谱/质谱联用(GC-MS),对古井贡酒中高温大曲进行分析,共定性出108种挥发性化合物。通过考察不同样品量下化合物的β值,在35和50 mg样品量下,建立了应用多次顶空固相微萃取(multiple headspace solid-phase microextraction,MHS-SPME)对醛酮类、酚类、含氮类、呋喃类、内酯类、萜烯类等46种化合物进行定量的方法。该方法回收率为76.83%~133.11%、最低检测限(limits of detection,LOD)低于103.818 ng/g、相对标准偏差(RSD%)小于21.34%,具有较好的灵敏度和重复性。实验结果表明MHS-SPME可用于大曲中这46种化合物的定量,化合物含量在(3645.79±442.43)^(6.32±1.03)ng/g之间。该方法为定量大曲中挥发性成分提供了新的思路,研究结果也为企业完善大曲质量评价体系提供了数据支持。

Headspace solid-phase microextraction(HS-SPME)combined with gas chromatography-mass spectrometry(GC-MS)was used to analyze the medium high temperature Daqu in Gujing Gongjiu,and a total of 108 volatile compounds were identified.By examining theβvalues of the compounds under different sample amounts,multiple headspace solid-phase microextraction(MHS-SPME)was applied to quantify the aldehydes and ketones,phenols,nitrogen,furans,lactones,terpenes at the 35 and 50 mg samples,and a total of 46 compounds were quantified.The recoveries of the method ranged from 76.83%~133.11%,the limits of detection(LOD)were lower than 103.818 ng/g,and the relative standard deviation(RSD%)were less than 21.34%,which showed the method had good sensitivity and repeatability.The experimental results showed that MHS-SPME could be applied to the quantitative analysis of these 46 compounds in Daqu.The contents of measured compounds ranged from(3645.79±442.43)to(6.32±1.03)ng/g.This method provided a new idea for quantifying the volatile components in Daqu,and the results also provided data support for the enterprise to improve the Daqu quality evaluation system.