HS-SPME-GC-MS法分析即墨黄酒陈酿过程中香气成分的变化
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摘要
即墨黄酒是采用黍米酿制的特色黄酒,其香气成分和陈酿过程中香气的变化目前研究较少。本研究采用顶空-固相微萃取(HS-SPME)结合气相色谱-质谱联用技术(GC-MS)分析即墨黄酒的挥发性香气成分。通过优化萃取探针、萃取温度、萃取时间以及NaCl添加量,确定即墨黄酒香气成分的最佳提取条件:ACAR/PDMS/DVB复合涂层的萃取探针在50℃条件下萃取60 min,NaCl添加量为0.15 g/mL。从2009年、2012年、2013年、2015年酒样中分别检测出16,15,15,19种香气物质。苯乙醇、苯乙酸乙酯、苯丙酸乙酯、丁二酸二乙酯在4份酒样中均有检出。苯乙醇和丁二酸二乙酯的相对含量随陈酿年份的增加逐年减少。2012年酒样中苯乙酸乙酯和苯丙酸乙酯的相对含量最高。
Jimo rice wine is made by husked millet but the researches of aroma composition and aging changes in the present study are less. The volatile compounds in Jimo rice wine made in husked millet were investigated by headspace solid phase microextraction(HS-SPME) coupled with gas chromatography-mass spectrometry(GC-MS). The microextraction fiber type, extraction time, extraction temperature and salt dosage were optimized. The best condition was that samples were heated at 50 ℃ for 60 min using ACAR/PDMS/DVB fiber, and the salt dosage was 0.15 g/mL. A total of 16, 15, 15 and 19 compounds were identified in the rice wine samples of 2009, 2012, 2013 and 2015 respectively.Phenethylalcohol, benzeneacetic acid ethyl ester, benzenepropanoic acid ethyl ester and diethyl succinate were identified in all the samples. The relative content of phenethylalcohol and diethyl succinate decreased with the increase of time.The relative content of benzeneacetic acid ethyl ester and benzenepropanoic acid ethyl ester in 2012 sample are the highest.
Jimo rice wine is made by husked millet but the researches of aroma composition and aging changes in the present study are less. The volatile compounds in Jimo rice wine made in husked millet were investigated by headspace solid phase microextraction(HS-SPME) coupled with gas chromatography-mass spectrometry(GC-MS). The microextraction fiber type, extraction time, extraction temperature and salt dosage were optimized. The best condition was that samples were heated at 50 ℃ for 60 min using ACAR/PDMS/DVB fiber, and the salt dosage was 0.15 g/mL. A total of 16, 15, 15 and 19 compounds were identified in the rice wine samples of 2009, 2012, 2013 and 2015 respectively.Phenethylalcohol, benzeneacetic acid ethyl ester, benzenepropanoic acid ethyl ester and diethyl succinate were identified in all the samples. The relative content of phenethylalcohol and diethyl succinate decreased with the increase of time.The relative content of benzeneacetic acid ethyl ester and benzenepropanoic acid ethyl ester in 2012 sample are the highest.
引文
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[22]经斌,王栋,徐岩,等.中国黄酒中若干重要风味物质嗅觉阈值的研究[J].食品工业科技,2012,33(6):135-142.
[23]汪建国,沈玉根,伟杰,等.我国黄酒研究现状与发展趋势[J].中国酿造,2012,31(11):15-20.
[24]盖禹含,辛秀兰,杨国伟,等.不同酵母发酵的蓝莓香成分GC-MS分析[J].食品科学,2010,31(4):171-174.
[25]王贞强.瑞引酿酒葡萄Granoir果实与葡萄酒品质研究[D].杨凌:西北农林科技大学,2005.
[26]郎召伟.泸型酒酿造过程中风味物质变化分析[D].无锡:江南大学,2015.
[27]HERNANDEZ-ORTE P,CERSOSIMO M,LOSCOSN,et al.The development of varietal aroma from non-floral grapes by yeasts of different genera[J].Food Chemistry,2008,107(3):1064-1077.
[28]李红蕾,冯涛,荣志伟.黄酒酿制过程中风味物质变化规律的研究[J].食品工业,2011,32(12):69-72.
[29]COMUZZO P,TAT L,TONIZZO A,et al.Yeast derivatives(extractsand autolysates)in winemaking:Release of volatile compounds and effects on wine aroma volatility[J].Food Chemistry,2006,99(2):217-230.
[30]张莉,王华.桑葚汽酒挥发性成分的气相色谱-质谱分析[J].蚕业科学,2010,36(1):152-156.
[31]石金飞.啤酒酿造过程中酯类物质影响因素的初步研究[D].无锡:江南大学,2008.
[32]韩笑,毛健,黄桂东.微量通气处理对黄酒陈华过程中风味物质和游离氨基酸的影响[J].食品科学,2013,34(3):123-127.
[33]褚小米,应维茂,申超.黄酒香气成分的影响因素分析[J].酿酒科技,2014(5):84-88.
[34]胡建,池国红,何喜红.黄酒发酵过程中主要香气成分的变化[J].酿酒科技,2007(12):60-64.
[35]郭翔,胡普信,徐岩.黄酒挥发性风味物质的研究[J].酿酒科技,2004(5):79-81.
[2]全国食品工业标准化技术委员会酿酒分技术委员会.GB/T 13662-2008中国标准书号[S].北京:中国标准出版社,2008.
[3]何伏娟,林秀芳,童忠东.黄酒生产工艺与技术[M].北京:化学工业出版社,2015.
[4]王家林,张颖,于秦峰.黄酒风味物质成分的研究进展[J].酿酒科技,2011(8):96-98.
[5]苏海荣.黄酒中挥发性风味物质的研究[D].青岛:青岛科技大学,2013.
[6]刘浩,赵生满,任贵兴.顶空固相微萃取结合气质联用分析小米黄酒与黍米黄酒的香气成分[J].酿酒科技,2015(1):115-123.
[7]CABREDO-PINILLOS S,CEDRON FERNANDEZT,SAENZ BARRIO C.Comparison of different extraction methods applied to volatile compounds in wine samples previous to the determination by gas chrpmatography[J].Analytical Letters,2004,37(14):3063-3084.[8张妮,肖作兵,于海燕,等.顶空固相微萃取-气质联用测得樱桃酒中的挥发性成分[J].食品科学,2011,32(10):97-102.
[9]LACUTEM P M,MESTERES M,SALA C,et,al.Solid-phasemicroextractionand gas chromatography olfactometryanalysis of successively diluted samples.a new approach of arom a extract dilution analysis applied to the characterization of wine aroma[J].Journal of Agricultural and Food Chemistry,2003,51(27):7861-7865.
[10]张明霞,赵旭娜,杨天佑,等.顶空固相微萃取分析白酒香气物质的条件优化[J].食品科学,2011,32(10):97-102.
[11]王洪燕,张万生,李美萍,等.GC-MS分析不同地区黄酒中的易挥发成分[J].酿酒科技,2015(9):115-121.
[12]朱潘炜.绍兴加饭黄酒风味物质指纹图谱的建立[D].杭州:浙江大学,2010.
[13]郑春亮,郑睿行,黄韬睿,等.黄酒香气成分的研究[J].生命科学仪器,2008(6):30-34.
[14]刘俊,徐岩,陈双,等.顶空-固相微萃取-气质联用技术快速测定黄酒中氨基甲酸乙酯的方法研究[J].食品工业科技,2012,33(4):60-63,69.
[15]王培璇,毛健,李晓钟,等.不同地区黄酒挥发性物质差异性分析[J].食品科学,2014,35(6):83-89.
[16]王志娟,张生万,赵景龙,等.竹叶青酒易挥发成分顶空固相微萃取-气相色谱-质谱分析[J].食品科学,2014,35(8):253-258.
[17]李春美,钟慧臻,郝菊芳,等.固相微萃取-气相色谱-质谱联用法分析荔枝汁贮藏过程中香气成分的变化[J].食品科学,2011,32(8):206-211.
[18]宋海燕.黄酒特征香气成分分析及特型黄酒开发研究[D].杭州:浙江农林大学,2013.
[19]HOWARD K L,MIKE J H,RIESEN R.Validation of a soid-phase microextraction method for headspace analysis of wine aroma components[J].American Joumal of Enology and Viticulture,2005,56(1):37-45.
[20]鲍忠定,许荣年.黄酒香气成分的分析[J].酿酒科技,1999(5):66-68.
[21]陈双,罗涛,徐岩,等.我国黄酒酵母和酿酒原料对黄酒中β-苯乙醇含量的影响[J].中国酿造,2009,28(4):23-26.
[22]经斌,王栋,徐岩,等.中国黄酒中若干重要风味物质嗅觉阈值的研究[J].食品工业科技,2012,33(6):135-142.
[23]汪建国,沈玉根,伟杰,等.我国黄酒研究现状与发展趋势[J].中国酿造,2012,31(11):15-20.
[24]盖禹含,辛秀兰,杨国伟,等.不同酵母发酵的蓝莓香成分GC-MS分析[J].食品科学,2010,31(4):171-174.
[25]王贞强.瑞引酿酒葡萄Granoir果实与葡萄酒品质研究[D].杨凌:西北农林科技大学,2005.
[26]郎召伟.泸型酒酿造过程中风味物质变化分析[D].无锡:江南大学,2015.
[27]HERNANDEZ-ORTE P,CERSOSIMO M,LOSCOSN,et al.The development of varietal aroma from non-floral grapes by yeasts of different genera[J].Food Chemistry,2008,107(3):1064-1077.
[28]李红蕾,冯涛,荣志伟.黄酒酿制过程中风味物质变化规律的研究[J].食品工业,2011,32(12):69-72.
[29]COMUZZO P,TAT L,TONIZZO A,et al.Yeast derivatives(extractsand autolysates)in winemaking:Release of volatile compounds and effects on wine aroma volatility[J].Food Chemistry,2006,99(2):217-230.
[30]张莉,王华.桑葚汽酒挥发性成分的气相色谱-质谱分析[J].蚕业科学,2010,36(1):152-156.
[31]石金飞.啤酒酿造过程中酯类物质影响因素的初步研究[D].无锡:江南大学,2008.
[32]韩笑,毛健,黄桂东.微量通气处理对黄酒陈华过程中风味物质和游离氨基酸的影响[J].食品科学,2013,34(3):123-127.
[33]褚小米,应维茂,申超.黄酒香气成分的影响因素分析[J].酿酒科技,2014(5):84-88.
[34]胡建,池国红,何喜红.黄酒发酵过程中主要香气成分的变化[J].酿酒科技,2007(12):60-64.
[35]郭翔,胡普信,徐岩.黄酒挥发性风味物质的研究[J].酿酒科技,2004(5):79-81.