2种芝麻香型白酒中香气活性成分分析
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摘要
应用液液萃取法结合气相色谱-质谱-嗅闻联用仪分析2种芝麻香型白酒(BTQ、YH)中香气活性成分。经保留指数、香气特征并结合标准品比对,BTQ和YH分别定性出挥发性化合物75种和68种;结合气相色谱-质谱-嗅闻联用通过芳香萃取物稀释分析分别嗅闻出香气活性化合物48种和46种,BTQ中香气稀释(flavor dilution,FD)因子值最大的是3-甲硫基丙醛(FD=6 561);YH中FD最大的是苯乙醇、3-甲基-1-丁醇、丁酸乙酯、戊酸乙酯(FD=2 187)。通过多种方法联用,对嗅闻到的51种香气活性成分和28种非嗅闻活性成分进行定量分析,并结合相关阈值进行香气活性值(odor activity value,OAV)分析,比较它们对整体香气的贡献程度,发现BTQ中有40种化合物OAV不小于1,YH中有36种化合物OAV不小于1,2种酒中香气贡献度最高的是己酸乙酯、3-甲基丁醛、丁酸乙酯、3-甲基丁酸乙酯。结合FD因子及OAV,对这2种芝麻香型白酒香气有重要贡献的化合物有己酸乙酯、丁酸乙酯和3-甲基丁醛。
The odor-active compounds in two brands(BTQ and YH) of Chinese sesame-flavor Baijius were extracted by liquid-liquid extraction and analyzed by gas chromatography-mass spectrometry-olfactometry(GC-MS-O). A total of 75 compounds in BTQ and 68 compounds in YH were identified by comparison of their retention indices(RI) and odor characteristics with those of reference standards. Among them, 48 odor-active compounds in BTQ and 46 in YH were further confirmed by GC-MS-O with aroma extract dilution analysis(AEDA). The highest flavor dilution(FD = 6 561) factor was determined for methional in BTQ. Phenethyl alcohol, 3-methyl-1-butanol, ethyl butanoate, and ethyl pentanoate had the highest FD factor(FD = 2 187) in YH. A total of 51 odor-active compounds and 28 compounds that were not detected by GC-MS-O were quantitated, and odor activity value(OAV) was used to rank their contributions to the overall aroma.The results of OAVs showed that there were 40 compounds with OAVs ≥ 1 in BTQ and 36 compounds with OAVs ≥ 1 in YH. It turned out that ethyl hexanoate, 3-methyl butanal, ethyl butanoate, and ethyl 3-methyl butanoate made the greatest contributions to the aroma of Chinese sesame-flavor Baijiu. Based on FD factors and OAVs, ethyl hexanoate, ethyl butanoate, 3-methyl butanoate made important contributions to the aroma of Chinese sesame-flavor Baijiu.
The odor-active compounds in two brands(BTQ and YH) of Chinese sesame-flavor Baijius were extracted by liquid-liquid extraction and analyzed by gas chromatography-mass spectrometry-olfactometry(GC-MS-O). A total of 75 compounds in BTQ and 68 compounds in YH were identified by comparison of their retention indices(RI) and odor characteristics with those of reference standards. Among them, 48 odor-active compounds in BTQ and 46 in YH were further confirmed by GC-MS-O with aroma extract dilution analysis(AEDA). The highest flavor dilution(FD = 6 561) factor was determined for methional in BTQ. Phenethyl alcohol, 3-methyl-1-butanol, ethyl butanoate, and ethyl pentanoate had the highest FD factor(FD = 2 187) in YH. A total of 51 odor-active compounds and 28 compounds that were not detected by GC-MS-O were quantitated, and odor activity value(OAV) was used to rank their contributions to the overall aroma.The results of OAVs showed that there were 40 compounds with OAVs ≥ 1 in BTQ and 36 compounds with OAVs ≥ 1 in YH. It turned out that ethyl hexanoate, 3-methyl butanal, ethyl butanoate, and ethyl 3-methyl butanoate made the greatest contributions to the aroma of Chinese sesame-flavor Baijiu. Based on FD factors and OAVs, ethyl hexanoate, ethyl butanoate, 3-methyl butanoate made important contributions to the aroma of Chinese sesame-flavor Baijiu.
引文
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[28]陈梦圆,刘学彬,汪平,等.产酯香功能菌对酱香型酒醅的影响[J].食品科学,2018,39(10):199-205.DOI:10.7506/spkx1002-6630-201810031.
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[30]沈怡方.白酒生产技术全书[M].北京:中国轻工业出版社,1998:11-15.
[31]王珍,周洋,李春丽,等.浅谈白酒中杂醇油的分析方法[J].酿酒科技,2017(6):77-79.DOI:10.13746/j.njkj.2017057.
[32]高年发.高效液相色谱法测定葡萄酒中的有机酸[J].酿酒,2004,31(1):67-69.DOI:10.3969/j.issn.1002-8110.2004.01.030.
[33]高传强.芝麻香型白酒风味物质及其生物活性研究[D].武汉:湖北工业大学,2017.
[34]余乾伟.传统白酒酿造技术[M].北京:中国轻工业出版社,2010.
[35]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
[36]陈双,徐岩.全二维气相色谱-飞行时间质谱法分析芝麻香型白酒中挥发性组分特征[J].食品与发酵工业,2017,43(7):207-213.DOI:10.13995/j.cnki.11-1802/ts.014825.
[37]SUN J Y,LI Q,LUO S,et al.Characterization of key aroma compounds in Meilanchun sesame flavor style baijiu by application of aroma extract dilution analysis,quantitative measurements,aroma recombination,and omission/addition experiments[J].RSC Advances,2018(42).DOI:10.1039/c8ra02727g.
[38]LAKE B G,PRICE R J,WALTERS D G,et al.Studies on the metabolism of the thiofurans furfuryl mercaptan and 2-methyl-3-furanthiol in rat liver[J].Food&Chemical Toxicology,2003,41(12):1761-1770.DOI:10.1016/S0278-6915(03)00213-8.
[2]刘涛.试论白酒的分类、生产工艺及其营养价值[J].酿酒,2018,45(3):21-22.DOI:10.3969/j.issn.1002-8110.2018.03.010.
[3]杨柳.中国白酒香型划分回顾与反思[J].酿酒科技,2016(5):115-116;120.DOI:10.13746/j.njkj.2016099.
[4]李大和.白酒香型融合的典型范例[J].酿酒,2008,35(3):3-6.DOI:10.3969/j.issn.1002-8110.2008.03.003.
[5]晓肖.2016中国芝麻香型酿造技术研讨会在洋河股份成功举办[J].酿酒,2017(1):109.DOI:10.3969/j.issn.1002-8110.2017.01.031.
[6]黄业立.试论芝麻香型白酒[J].酿酒科技,2007(10):116-119.DOI:10.3969/j.issn.1001-9286.2007.10.033.
[7]沈怡方.芝麻香型白酒的生产实践总结[J].酿酒,2017,44(1):3-6.DOI:10.3969/j.issn.1002-8110.2017.01.001.
[8]郑杨,赵纪文,张锋国,等.扳倒井芝麻香型白酒香成分分析[J].食品科学,2014,35(4):60-65.DOI:10.7506/spkx1002-6630-201404013.
[9]胡国栋,陆久瑞,蔡心尧,等.芝麻香型白酒特征组分的分析研究[J].酿酒科技,1994(4):75-77.DOI:10.13746/j.njkj.1994.04.036.
[10]武金华,孙启栋,姜淑芬,等.对生力源芝麻香型白酒成分的分析及探讨[J].酿酒科技,2009(6):65-66.DOI:10.13746/j.njkj.2009.06.015.
[11]张媛媛,孙金沅,张国锋,等.扳倒井芝麻香型白酒中含硫风味成分的分析[J].中国食品学报,2012,12(12):173-179.DOI:10.16429/j.1009-7848.2012.12.027.
[12]张媛媛,孙金沅,张锋国,等.芝麻香型白酒中含硫风味组分的分析[J].中国食品学报,2014,14(5):218-225.DOI:10.16429/j.1009-7848.2014.05.005.
[13]ZHENG Y,SUN B G,ZHAO M M,et al.Characterization of the key odorants in Chinese Zhima aroma-type Baijiu by gas chromatographyolfactometry,quantitative measurements,aroma recombination,and omission studies[J].Journal of Agricultural and Food Chemistry,2016,64(26):5367-5374.DOI:10.1021/acs.jafc.6b01390.
[14]SHA S,CHEN S,QIAN M,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].Journal of Agricultural and Food Chemistry,2017,65(1):123-131.DOI:10.1021/acs.jafc.6b04242.
[15]SUN J,ZHAO D,ZHANG F,et al.Joint direct injection and GC-MSchemometric approach for chemical profile and sulfur compounds of sesame-flavor Chinese Baijiu(Chinese liquor)[J].European Food Research and Technology,2018,244(1):145-160.DOI:10.1007/s00217-017-2938-7.
[16]GAO W,FAN W,XU Y.Characterization of the key odorants in light aroma type Chinese liquor by gas chromatography-olfactometry,quantitative measurements,aroma recombination,and omission studies[J].Journal of Agricultural and Food Chemistry,2014,62(25):5796-804.DOI:10.1021/jf501214c.
[17]李研科,王国明,孙文,等.HS-SPME-GC-MS法分析酱香型“山庄老酒”香气成分[J].酿酒科技,2018(4):112-117.DOI:10.13746/j.njkj.2017260.
[18]郑杨.芝麻香型白酒关键香气成分研究[D].广州:华南理工大学,2017.
[19]周庆云.芝麻香型白酒风味物质研究[D].无锡:江南大学,2015.
[20]CZERNY M,CHRISTLBAUER M,et al.Re-investigation on odour thresholds of key food aroma compounds and development of an aroma language based on odour qualities of defined aqueous odorant solutions[J].European Food Research&Technology,2008,228(2):265-273.DOI:10.1007/s00217-008-0931-x.
[21]范文来.白酒79个风味化合物嗅觉阈值测定[J].酿酒,2011,38(4):80-84.DOI:10.3969/j.issn.1002-8110.2011.04.034.
[22]FAN W,QIAN M C.Characterization of aroma compounds of Chinese “Wuliangye” and “Jiannanchun” liquors by aroma extract dilution analysis[J].Journal of Agricultural&Food Chemistry,2006,54(7):2695-2704.DOI:10.1021/jf052635t.
[23]SCHIEBERLE P.Chapter 17:new developments in methods for analysis of volatile flavor compounds and their precursors[J].Characterization of Food,1995,65(7):403-431.
[24]BIANCHI F,CARERI M,MANGIA A,et al.Retention indices in the analysis of food aroma volatile compounds in temperatureprogrammed gas chromatography:database creation and evaluation of precision and robustness[J].Journal of Separation Science,2007,30(4):563-572.DOI:10.1002/jssc.200600393.
[25]ZHAO D,SHI D,SUN J,et al.Characterization of key aroma compounds in Gujinggong Chinese Baijiu by gas chromatographyolfactometry,quantitative measurements,and sensory evaluation[J].Food Research International,2018,105:616-627.DOI:10.1016/j.foodres.2017.11.074.
[26]陶新功.从四大酯类含量分析糟烧白酒[J].中国酿造,2013,32(9):120-122.DOI:10.3969/j.issn.0254-5071.2013.09.031.
[27]张丽敏.中国白酒与风味物质[J].酿酒科技,2002(3):41-42.DOI:10.3969/j.issn.1001-9286.2002.03.011.
[28]陈梦圆,刘学彬,汪平,等.产酯香功能菌对酱香型酒醅的影响[J].食品科学,2018,39(10):199-205.DOI:10.7506/spkx1002-6630-201810031.
[29]周庆云,范文来,徐岩.景芝芝麻香型白酒重要挥发性香气成分研究[J].食品工业科技,2015,36(16):62-67.DOI:10.13386/j.issn1002-0306.2015.16.004.
[30]沈怡方.白酒生产技术全书[M].北京:中国轻工业出版社,1998:11-15.
[31]王珍,周洋,李春丽,等.浅谈白酒中杂醇油的分析方法[J].酿酒科技,2017(6):77-79.DOI:10.13746/j.njkj.2017057.
[32]高年发.高效液相色谱法测定葡萄酒中的有机酸[J].酿酒,2004,31(1):67-69.DOI:10.3969/j.issn.1002-8110.2004.01.030.
[33]高传强.芝麻香型白酒风味物质及其生物活性研究[D].武汉:湖北工业大学,2017.
[34]余乾伟.传统白酒酿造技术[M].北京:中国轻工业出版社,2010.
[35]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
[36]陈双,徐岩.全二维气相色谱-飞行时间质谱法分析芝麻香型白酒中挥发性组分特征[J].食品与发酵工业,2017,43(7):207-213.DOI:10.13995/j.cnki.11-1802/ts.014825.
[37]SUN J Y,LI Q,LUO S,et al.Characterization of key aroma compounds in Meilanchun sesame flavor style baijiu by application of aroma extract dilution analysis,quantitative measurements,aroma recombination,and omission/addition experiments[J].RSC Advances,2018(42).DOI:10.1039/c8ra02727g.
[38]LAKE B G,PRICE R J,WALTERS D G,et al.Studies on the metabolism of the thiofurans furfuryl mercaptan and 2-methyl-3-furanthiol in rat liver[J].Food&Chemical Toxicology,2003,41(12):1761-1770.DOI:10.1016/S0278-6915(03)00213-8.