酱香型白酒微量挥发性香气成分检测方法的建立及应用  

Establishment and application of a method for determination of trace volatile aroma components in sauce-flavorBaijiu

作　　者：王金龙 朱晓春 尤小龙 田栋伟 陆伦维 胡建锋 WANG Jinlong;ZHU Xiaochun;YOU Xiaolong;TIAN Dongwei;LU Lunwei;HU Jianfeng(Guizhou Xijiu Co.,Ltd.,Zunyi 564622,China)

机构地区：[1]贵州习酒股份有限公司,贵州遵义564622

出　　处：《中国酿造》2025年第4期267-275,共9页China Brewing

基　　金：贵州省科技计划项目(黔科合成果[2023]145)。

摘　　要：该研究应用分散液液微萃取(DLLME)结合气相色谱-质谱(GC-MS)技术建立酱香型白酒微量挥发性香气成分的检测方法。采用该方法对仁怀和习水产区酱香型白酒样品中的微量挥发性香气成分进行检测,并基于检测结果进行聚类分析和偏最小二乘-判别分析(PLS-DA)。结果表明,采用DB-FFAP毛细管色谱柱(60 m×0.25 mm×0.25μm),以乙醚-正己烷(1∶1)为萃取剂萃取2 min,在此条件下可以有效的定性定量酱香型白酒中59种微量挥发性香气成分,各成分在检测范围内呈现出良好的线性关系(相关系数R^(2)为0.9963~0.9999),检出限为0.15~2.43μg/L,定量限为0.28~6.07μg/L,加标回收率为93.00%~103.94%,精密度试验(n=6)结果的相对标准偏差(RSD)为0.34%~6.30%,说明该方法的精密度和回收率较好,能满足酱香型白酒59种微量挥发性香气成分的检测需求。根据59种微量挥发性香气成分可以有效的对仁怀和习水产区酱香型白酒样品进行区分,根据变量重要性投影(VIP)值>1筛选得到二甲基二硫、三甲基吡嗪等8种主要差异微量香气成分。A method for the determination of trace volatile aroma components in sauce-flavor(Jiangxiangxing)Baijiu was developed by dispersed liquid-liquid microextraction(DLLME)combined with gas chromatography-mass spectrometry(GC-MS).The trace volatile aroma components in the sauce-flavor Baijiu samples from Renhuai and Xishui producing areas were detected,and cluster analysis and partial least squares-discriminant analysis(PLS-DA)were carried out based on the detection results.The results showed that the DB-FFAP capillary column(60 mx0.25 mmx0.25μm)was adopted,and extraction for 2 min with ether/n-hexane(1:1)as the extractant.Under these conditions,59 trace volatile aroma components in sauce-flavor Baijiu could be qualitatively and quantitatively determined effectively,and each component showed a good linear relationship within the detection range.The correlation coefficient(R^(2))of this method was 0.9963-0.9999,the detection limit was 0.15-2.43μg/L,the quantification limit was 0.28-6.07μg/L,the spiked recovery rates were 93.00%-103.94%,and the relative standard deviation(RSD)of precision tests(n=6)was 0.34%-6.30%,which indicated that the precision and recovery rates of this method were good and could meet the detection requirements of 59 trace volatile aroma components in sauce-flavor Baijiu.The sauce-flavor Baijiu samples from Renhuai and Xishui producing areas could be effectively distinguished according to 59 trace volatile aroma components.8 kinds of main difference trace aroma components such as dimethyl disulfide and trimethyl pyrazine,could be screened according to variable importance in the projection(VIP)value>1.

关 键 词：酱香型白酒 微量挥发性香气成分 分散液液微萃取 气相色谱-质谱 方法学考察 偏最小二乘-判别分析 

分 类 号：O657.7[理学—分析化学]