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

作　　者：王松 陈璐[1,2] 刘国英 孙金沅[1,2] 张燕燕 李贺贺[1,2] 孙宝国[1,2] Wang Song;Chen Lu;Liu Guoying;Sun Jinyuan;Zhang Yanyan;Li Hehe;Sun Baoguo(Beijing Laboratory of Food Quality and Safety,Beijing Technology and Business University,Beijing 100048,China;Beijing Key Laboratory of Food Flavor Chemistry,Beijing Technology and Business University,Beijing 100048,China;Anhui Gujing Group Co.Ltd.,Bozhou 236000,Anhui,China;Department of Flavor Chemistry,University of Hohenheim,Stuttgart,70599,Germany)

机构地区：[1]食品质量与安全北京实验室,北京工商大学,北京100048 [2]北京市食品风味化学重点实验室,北京工商大学,北京100048 [3]安徽古井贡酒股份有限公司,安徽亳州236000 [4]霍恩海姆大学风味化学系,德国斯图加特70599

出　　处：《精细化工》2020年第2期346-355,390,共11页Fine Chemicals

基　　金：国家自然科学基金(31972193);国家重点研发计划(2016YFD0400500).

摘　　要：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.

关 键 词：多次顶空固相微萃取 大曲 挥发性化合物 定量 气相色谱-质谱联用 食品与饲料用化学品 

分 类 号：O657.63[理学—分析化学] TS261.11[理学—化学]