| With the development of society,people’s living standard was increasing,more and more consumers were favored in the old year liquor with its rare,expensive,unique flavor and other characteristics.It is important to explore the volatiles in different quality liquor and analyze each sample,which is of great significance to regulate the circulation of old year liquors.In this paper,five samples which were the 5 years,the 8 years,the 16 years,the 26 years and the Gift of Gujinggong Nianfenyuanjiang series were used to study the volatiles with different pretreatment methods combined with different detection techniques.The paper aimed to provide data support for improving the quality of Chinese Baijiu production and the technology.The main contents of this study were as follows:(1)Gas chromatography-mass spectrometry(GC-MS)combined with gas chromatography-olfactory-mass spectrometry(GC-O-MS)was used to study the effects with direct injection(DI).There were totally 48 kinds of volatiles detected by GC-MS in five samples,and 33 kinds of volatiles were identified on the 8 years baijiu by GC-O-MS.The contribution of them was determined based on aroma extraction dilution analysis(AEDA)and FD factors,hexanoic acid,ethyl hexanoate,ethyl 3-phenylpropionate(FD factor>1024),butyric acid(FD factor = 512)made great influence on the 8 years sample.(2)Gas chromatography-mass spectrometry(GC-MS)combined with gas chromatography-olfactory-mass spectrometry(GC-O-MS)was used to study the effects with liquor-liquor extraction(LLE).Retention index,MS,standard matching and olfactory were four methods combined to qualitative the volatiles.A total of 71 compounds were identified by GC-MS in 5 samples,and 50 kinds of volatiles in the 8 years baijiu were identified by GC-O-MS.(3)The internal standard method was used to quantify 48 kinds of compounds which were qualitative by direct injection(DI),and the mode was GC-MS/SIM.The detection limit of this method was low,the linearity was good and the sensitivity was high.The quantitative results combined with the OAV values determined ethyl hexanoate,ethyl octanoate,ethyl butyrate,ethyl pentanoate and butyric acid were more important of aroma contribution.(4)The 50 kinds of volatiles identified by liquid-liquid extraction combined with GC-O-MS were quantified by internal standard method.The mode was GC-MS / SIM.The detection limit was 5.00 ~ 2500.00 μg/L,the recovery rate was between 90% and 110%,the linear correlation coefficient R2 was more than 0.99,and the relative standard deviation(RSD)was less than 5%,which showed the method had high sensitivity,good precision,low detection limit and good linearity.For the quantitative results,the OAV values were used to determine the characteristic volatiles of five samples,and its contribution to the degree of flavor in-depth analysis. |