顶空固相微萃取-气相色谱质谱法测定馥郁香型白酒中的挥发性香气成分

Determination of volatile aroma components in Fuyu flavor liquor by head space-solid phase microextraction with gas chromatography-mass spectrometry

中文关键词:  馥郁香型白酒  顶空固相微萃取  气相色谱质谱联用  风味物质

英文关键词:Fuyu flavor liquor  head space-solid phase microextraction  gas chromatography-mass spectrometry  flavor compounds

中文摘要:

      目的 建立顶空固相微萃取-气相色谱质谱法(head space-solid phase microextraction, HS-SPME)测定白酒中风味物质的分析方法。方法 以馥郁香型白酒为主要研究对象, 采用固相微萃取和气相色谱-质谱联用法(gas chromatography-mass spectrometry, GC-MS)分析馥郁香型白酒中的风味成分, 确定萃取头种类, 利用正交试验对萃取时间、萃取温度、解析时间、解析温度进行优化。结果 馥郁香型白酒风味物质的顶空固相微萃取-气相色谱质谱法最佳条件为: 选用50/30 μm DVB/CAR/PDMS Stableflex(grey)固相微萃取头, 稀释倍数1:2(V:V), 加入2 g氯化钠, 萃取时间40 min、萃取温度为75 ℃、解析时间5 min、解析温度290 ℃。对馥郁香型白酒的风味物质分析得到74种成分, 分别为酯类50种、醇类8种、酸类6种、酮类3种、酚类2种、醛类2种、含硫含氮化合物3种。方法相对标准偏差(relative standard deviation, RSD)为2.9%~15.7%。利用优化条件对酱香型、浓香型、清香型白酒进行分析, 分别得到64种、52种和44种香气成分。有29种香气成分为馥郁香型白酒特有。馥郁香型白酒与酱香型、浓香型、清香型白酒香气成分在含量上不同, 馥郁香型白酒中己酸乙酯、己酸己酯含量明显高于酱香型白酒、浓香型白酒和清香型白酒。结论 本研究建立的方法快速、简单, 可用于白酒风味物质的检测。

英文摘要:

      Objective To establish a method for the determination of flavor compounds from Fuyu flavor liquor by head space-solid phase microextraction (HS-SPME) with gas chromatography-mass spectrometry (GC-MS). Methods With the Fuyu flavor liquor as main object, volatile compounds were qualitatively determined by headspace solid-phase microextraction (HS-SPME) and gas chromatography coupled with mass spectrometry (GC-MS). The type of extraction head was chosed, the optimal SPME extraction condition was determined by orthogonal array design method. Results The optimum conditions for the headspace solid phase microextraction- gas chromatography mass spectrometry of flavor compounds in Fuyu flavor liquor were as follows: The 50/30 μm DVB/CAR/PDMS Stableflex (grey)extraction head was selected, dilution ratio was 1:2, NaCl was 2 g, extraction time was 40 min, extraction temperature was 75 ℃, desorption time was 5 min, and desorption temperature was 290 ℃. A total of 74 components, including 50 esters, 8 alcohols, 6 acids, 3 ketones, 2 phenols, 2 aldehydes and 3 sulfur and nitrogen compounds, were obtained from the Fuyu flavor liquor. The relative standard deviations (RSDs) were 2.9%~15.7%. The optimum conditions were used to analyze Maotai flavor liquor, Luzhou flavor liquor and Qingxiang flavor liquor, and 64, 52 and 44 aroma components were obtained, respectively. Among them, 29 aroma components were unique to Fuyu flavor liquor. The differences in the content of Fuyu flavor liquor and the aroma components of Maotai, Luzhou and Qingxiang liquors were found out, and the content of hexanoic acid, ethyl ester and hexanoic acid, hexyl ester in Fuyu liquor was significantly higher than that of Maotai flavor liquor, Luzhou flavor liquor and Qing flavor liquor. Conclusion This method is rapid and simple, which can be used for the detection of flavor compounds in liquor.