采用液液萃取和顶空固相微萃取两种前处理方法,结合气相色谱质谱联用及保留指数法,首次分析了酱香型盐菜味缺陷酒的风味物质组成。采用多级鉴定策略,在酱香型盐菜味缺陷酒中检测出76种化合物,其中醇类物质9种、醛酮类物质7种、酸类物质10种、酯类物质31种、酚类物质3种、内酯类物质3种、呋喃类物质5种、含氮化合物4种、含硫化合物1种、烃类及其他类物质3种,并检测出未在白酒中报道过的2,4-二叔丁基苯酚和2,2-亚甲基双呋喃。液液萃取和顶空固相微萃取两种方法的萃取物质具有一定倾向性,配合使用有更宽的检测范围。酱香型白酒表现出盐菜味缺陷,很有可能是由多种化合物相互作用引起。缺陷酒中化合物的分析检测,为后续研究奠定了基础。
The volatile compounds from pickled mustard (Brassica juncea) like off-flavor Maotai-flavor liquor were qualitatively analyzed by liquid-liquid extraction (LLE) and HS-SPME combined with GC-MS for the first time. There were 76 volatile compounds identified in total, including 9 alcohols, 7 aldehydes and ketones, 10 acids, 31 esters, 3 phenols, 3 lactones, 5 furans, 4 nitrogen-containing compounds, 1 sulfur-containing compound and 3 hydrocarbons and other substances. In addition, 2,4-ditert-butyl phenol and 2,2-methylenedifuran that had not been reported in liquor were detected. It was concluded that co-application of LLE and HS-SPME had a wider detection range, and the interactions between various compounds may result in off-flavor of the Maotai-flavor liquor. The analysis and detection of the compounds in the defective liquor lays a foundation on subsequent researches.
[1] NIU Y, CHEN X, XIAO Z, et al. Characterization of aroma-active compounds in three Chinese Moutai liquors by gas chromatography-olfactometry, gas chromatography-mass spectrometry and sensory evaluation[J]. Natural Product Research, 2016, 31(8): 1.
[2] ZHAO T, CHEN S, LI H, et al. Identification of 2-Hydroxymethyl-3,6-diethyl-5-methylpyrazine as a key retronasal burnt flavor compound in soy sauce aroma type Baijiu using sensory-guided isolation assisted by multivariate data analysis[J]. Journal of Agricultural and Food Chemistry,2018, 66: 10 496-10 505.
[3] 张灿. 中国白酒中异嗅物质研究[D]. 无锡:江南大学, 2013.
[4] CHEN S, SHA S, QIAN M, et al. Characterization of volatile sulfur compounds in Moutai liquors by headspace solid-phase microextraction gas chromatography-pulsed flame photometric detection and odor activity value[J]. Journal of Food Science, 2017, 82(12): 2 816-2 822.
[5] DING X, WU C, HUANG J, et al. Characterization of interphase volatile compounds in Chinese Luzhou -flavor liquor fermentation cellar analyzed by head space-solid phase micro extraction coupled with gas chromatography mass spectrometry (HS-SPME/GC/MS)[J]. LWT-Food Science and Technology, 2016, 66:124-133.
[6] 王尹叶, 范文来,徐岩. 白酒中挥发性苦涩味物质的提取和分离[J]. 食品与发酵工业, 2018, 44(6): 240-244.
[7] 杨亮, 占杨杨,魏刚,等.基于气质联用法的两种香型白酒挥发性成分差异分析[J]. 中国酿造, 2018, 37(10): 76-81.
[8] 崔宗岩, 王飞,刘晓茂,等. 乙基化衍生-气相色谱-串联质谱法测定葡萄酒中3种丁基锡:液液萃取和固相微萃取的比较[J]. 分析试验室, 2016, 35(10): 1 161-1 166.
[9] 唐柯, 王茜,周霞,等. 石榴酒发酵过程中香气动态变化规律[J]. 食品与发酵工业, 2019, 45(6): 197-202;214.
[10] WANG L, HU G, LEI L, et al. Identification and aroma impact of volatile terpenes in Moutai liquor[J]. International Journal of Food Properties, 2016, 19(6): 18.
[11] VERNON E CATES, CLIFTON E MELOAN. Separation of sulfones by gas chromatography[J]. J Chromatogr, 1963, 11(4): 472-478.
[12] 范文来, 徐岩. 白酒香气物质研究的方法学[J]. 食品科学技术学报, 2018, 36(3): 1-10.
[13] ZHU Wenqi. Identification of compounds responsible for the characteristic “soy sauce” flavor of traditional Chinese liquor[D]. University of Illinois at Urbana-Champaign, 2018: 5-6.
[14] PENG Q, RUI D, XUN S, et al. Determination of volatile phenols in Chinese liquors by high-performance liquid chromatography associated with β-cyclodextrin and a protective barrier layer[J]. Flavour & Fragrance Journal, 2013, 28(3): 137-143.
[15] SHA S, CHEN S, QIAN M C, et al. Characterization of the typical potent odorants in Chinese Roasted Sesame-Like Flavor Type Liquor by headspace solid phase microextraction-aroma extract dilution analysis, with special emphasis on sulfur-containing odorants[J]. J Agric Food Chem, 2016, 65(1): 123-131.
[16] 沙莎. 白酒中挥发性含硫化合物及其风味贡献研究[D]. 无锡:江南大学, 2017.
[17] WANG X, FAN W, XU Y. Comparison on aroma compounds in Chinese soy sauce and strong aroma type liquors by gas chromatography-olfactometry, chemical quantitative and odor activity values analysis[J]. European Food Research & Technology, 2014, 239(5): 813-825.
[18] 赵书圣, 范文来,徐岩,等. 酱香型白酒生产酒醅中呋喃类物质研究[J]. 中国酿造, 2008, 27(21): 10-13.
[19] FAN W, XU Y, HAN Y. Quantification of volatile compounds in Chinese Ciders by stir bar sorptive extraction (SBSE) and gas chromatography-mass spectrometry (GC-MS)[J]. J Sci Food Agric, 2011, 91(7): 1 187-1 198.
[20] FAN W, XU Y, ZHANG Y. Characterization of pyrazines in some Chinese liquors and their approximate concentrations[J]. Journal of Agricultural & Food Chemistry, 2007, 55(24): 9 956-62.
[21] ZHU S, LU X, JI K, et al. Characterization of flavor compounds in Chinese liquor Moutai by comprehensive two-dimensional gas chromatography/time-of-flight mass spectrometry[J]. Analytica Chimica Acta, 2007, 597(2): 340-348.
