GC-MS/SIM法检测103种白酒中6种酚类化合物
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摘要
酚类化合物是白酒中重要的呈香呈味物质和有益成分,为检测其在不同白酒中的含量,本文采用直接进样结合气相色谱-质谱/选择离子扫描(GC-MS/SIM)对103种白酒中常见的4-甲基愈创木酚、苯酚、4-乙基愈创木酚、4-甲基苯酚、4-乙基苯酚和香兰素的含量进行检测。结果表明,该方法回收率在81.8%～115.6%之间,精密度均小于5%;在检测范围内具有良好的线性关系(R2>0.98),检出限为0.14～0.55μg/L,定量限为0.35～1.49μg/L。应用该方法对103种白酒的检测结果表明,不同香型白酒中不同酚类化合物含量差异较大,浓香型和芝麻香型白酒中相对含量较高,其中一种浓香型白酒样品中6种酚类物质总含量最高,为6.21 mg/L。
Phenolic compounds are important aroma compounds and beneficial ingredients in Baijiu, in order to detect and determine their content in different Chinese Baijiu, 4-methylguaiacol, phenol, 4-ethylguaiacol, 4-methylphenol,4-ethylphenol and vanillin of 103 kinds of Chinese Baijiu were quantified by direct injection combined with gas chromatography-mass spectrometry(GC-MS)/selective ion monitoring(SIM). The result showed: the average recovery of the method was between 81.8% and 115.6%, and RSD was all less than 5%, the method had good linearity(R2>0.98), the limit of detection(LOD) was from 0.14 to 0.55 μg/L, the limit of quantification was from 0.35 to 1.49 μg/L. The results showed that the contents of phenolic compounds varied greatly in different aroma types of Chinese Baijiu, the contents of phenolic compounds were higher in strong aroma type and zhima aroma-type Baijiu, and the highest content of phenolic compounds was 6.21 mg/L which was observed from strong aroma type Baijiu.
Phenolic compounds are important aroma compounds and beneficial ingredients in Baijiu, in order to detect and determine their content in different Chinese Baijiu, 4-methylguaiacol, phenol, 4-ethylguaiacol, 4-methylphenol,4-ethylphenol and vanillin of 103 kinds of Chinese Baijiu were quantified by direct injection combined with gas chromatography-mass spectrometry(GC-MS)/selective ion monitoring(SIM). The result showed: the average recovery of the method was between 81.8% and 115.6%, and RSD was all less than 5%, the method had good linearity(R2>0.98), the limit of detection(LOD) was from 0.14 to 0.55 μg/L, the limit of quantification was from 0.35 to 1.49 μg/L. The results showed that the contents of phenolic compounds varied greatly in different aroma types of Chinese Baijiu, the contents of phenolic compounds were higher in strong aroma type and zhima aroma-type Baijiu, and the highest content of phenolic compounds was 6.21 mg/L which was observed from strong aroma type Baijiu.
引文
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[5]周恒刚.4-乙基愈创木酚[J].酿酒,1989(6):7-9.
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[14]付博,张吉苹,姜晖,等.基于脂肪酸的漂浮液滴固化分散液液微萃取-高效液相色谱法联用测定酒类样品中的4-乙基苯酚和4-乙基愈创木酚[J].色谱,2016,34(9):895-900.
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[17]孙啸涛,王宗元,刘淼,等.涡旋辅助液液微萃取结合GC-MS法检测67种白酒中四甲基吡嗪、4-甲基愈创木酚和4-乙基愈创木酚[J].食品科学,2017,38(18):73-79.
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[19]SUN J,ZHAO D,ZHANG F,et al.Joint direct injection and GC-MS chemometric approach for chemical profile and sulfur compounds of sesamearoma Chinese Baijiu(Chinese liquor)[J].European Food Research and Technology,2018,244(1):145-160.
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[21]霍嘉颖,黄明泉,孙宝国,等.中国白酒中功能因子研究进展[J].酿酒科技,2017(9):17-23.
[22]ZHAO D,SUN J,SUN B,et al.Intracellular antioxidant effect of vanillin,4-methylguaiacol and 4-ethylguaiacol:three components in Chinese Baijiu[J].Royal Society Chemistry Advances,2017,7(73):46395-46405.
[2]傅玉书,胡国栋,龚书宝.气相色谱法分析白酒的非挥发性酚类化合物[J].色谱,1985(S1):111-115,283.
[3]孙宝国,李贺贺,胡萧梅,等.健康白酒的发展趋势[J].中国食品学报,2016,16(8):1-6.
[4]CERDAN T G,MOZAZ S R,AZPILICUETA C AVolatile composition of aged wine in used barrels of French oak and of American oak[J].Food Research International,2002,35(7):603-610.
[5]周恒刚.4-乙基愈创木酚[J].酿酒,1989(6):7-9.
[6]范文来,徐岩.白酒79个风味化合物嗅觉阈值测定[J].酿酒,2011,38(4):80-84.
[7]FAN W,QIAN M C.Characterization of aroma compounds of Chinese“Wuliangye”and“Jiannanchun”liquors by aroma extract dilution analysis[J].Journal of Agricultural and Food Chemistry,2006,54(7):2695-2704.
[8]LOURIERO V,MALFEITO-FERREIRA M.Spoilage yeasts in the wine industry[J].International Journal of Food Microbiology,2003,86(1/2):23-50.
[9]黄蕴利,黄永光,郭旭.白酒中的主要生物活性功能成分研究进展[J].食品工业科技,2016,37(15):375-379.
[10]FAN W,QIAN M C.Identification of aroma compounds of Chinese“Yanghe Daqu”liquor by normal phase chromatography fractionation followed by gas chromatography/olfactometry[J].Aroma and Fragrance Journal,2006,21(2):333-342.
[11]朱燕,范文来,徐岩.应用DI-SPME和GC-MS分析白酒中游离挥发性酚类化合物[J].食品与发酵工业,2010,36(10):138-143.
[12]寻思颖,董睿,彭黔荣,等.高效液相色谱法测定酱香型白酒中挥发性酚类物质[J].食品科学,2012,33(24):239-243.
[13]吴婷婷,朱双良,孙惜时,等.梅兰春芝麻香酒的健康因子分析[J].酿酒科技,2013(8):125-130.
[14]付博,张吉苹,姜晖,等.基于脂肪酸的漂浮液滴固化分散液液微萃取-高效液相色谱法联用测定酒类样品中的4-乙基苯酚和4-乙基愈创木酚[J].色谱,2016,34(9):895-900.
[15]WU J,ZHENG Y,SUN B,et al.The occurrence of propyl lactate in Chinese Baijius(Chinese Liquors)detected by direct injection coupled with Gas Chromatography-Mass Spectrometry[J].Molecules,2015,20(10):19002-19013.
[16]赵东瑞,柳金龙,张锋国,等.GC-MS/SIM内标法定量分析两种类型酒中的3-甲硫基丙醇[J].中国食品学报,2016,16(5):196-204.
[17]孙啸涛,王宗元,刘淼,等.涡旋辅助液液微萃取结合GC-MS法检测67种白酒中四甲基吡嗪、4-甲基愈创木酚和4-乙基愈创木酚[J].食品科学,2017,38(18):73-79.
[18]ZHENG Y,SUN B,ZHAO M,et al.Characterization of the key odorants in Chinese Zhima AromaType Baijiu by gas chromatography-olfactometry,quantitative measurements,aroma recombination,and omission studies[J].Journal of Agricultural and Food Chemistry,2016,64(26):5367-5374.
[19]SUN J,ZHAO D,ZHANG F,et al.Joint direct injection and GC-MS chemometric approach for chemical profile and sulfur compounds of sesamearoma Chinese Baijiu(Chinese liquor)[J].European Food Research and Technology,2018,244(1):145-160.
[20]刘博.浓香型白酒中窖泥异味物质4-甲基苯酚的产生机制研究[D].无锡:江南大学,2016.
[21]霍嘉颖,黄明泉,孙宝国,等.中国白酒中功能因子研究进展[J].酿酒科技,2017(9):17-23.
[22]ZHAO D,SUN J,SUN B,et al.Intracellular antioxidant effect of vanillin,4-methylguaiacol and 4-ethylguaiacol:three components in Chinese Baijiu[J].Royal Society Chemistry Advances,2017,7(73):46395-46405.