液液微萃取结合气质联用技术分析高温大曲中风味物质  

Analysis of flavor compounds in high-temperature Daqu by liquid-liquid microextraction combinedwith gas chromatography-mass spectrometry

作　　者：杨理章 倪德让 杨玉波 杨帆 王莉 YANG Lizhang;NI Derang;YANG Yubo;YANG Fan;WANG Li(Kweichow Moutai Co.,Ltd.,Zunyi 564501,China;Kweichow Moutai Group Co.,Ltd.,Zunyi 564501,China)

机构地区：[1]贵州茅台酒股份有限公司,贵州遵义564501 [2]中国贵州茅台酒厂(集团)有限责任公司,贵州遵义564501

出　　处：《中国酿造》2022年第8期223-228,共6页China Brewing

基　　金：遵义市科技计划项目(遵市科合R&D(2020)30号)。

摘　　要：该研究建立液液微萃取(LLME)结合气相色谱-质谱(GC-MS)联用技术分析高温大曲中风味物质的方法,并优化前处理条件。结果表明,最佳前处理条件为:称取大曲样品15 g;提取溶剂为30 m L体积分数40%乙醇;提取方式为先以转速450 r/min摇床振摇15 min,再经过120 W超声仪超声提取5 min;萃取剂及用量为乙醚2 m L;漩涡振荡时间40 s。在此优化前处理条件下,GC-MS共检出25种风味物质,其中酸类7种、芳香族6种、吡嗪类5种、杂环类2种、醇类2种、以及酚类、酮类和含硫化合物各1种。各风味物质标准曲线的线性关系良好,相关系数R2均≥0.99,精密度试验结果相对标准偏差(RSD)≤7.26%,加标回收率为80.25%~119.26%,方法检出限为0.13~50.17μg/kg,定量限为0.44~167.22μg/kg。该方法精密度及准确度良好,可满足大曲风味物质准确定量分析要求。Flavor compounds in high-temperature Daqu were analyzed by liquid-liquid microextraction(LLME)combined with GC-MS,and the pretreatment conditions were optimized.The results showed that the optimum pretreatment conditions were as follows:15 g Daqu was dissolved in 30 ml ethanol with volume fraction 40%,then shaken on the shaking table at 450 r/min for 15 min and ultrasonic extracted at 120 Wfor 5 min,the extraction agent and dosage was ether 2 ml,and the vortex oscillation time was 40 s.Based on the optimal pretreatment conditions,a total of 25 flavor compounds were detected,including 7 acids,6 aromatics,5 pyrazines,2 heterocycles,2 alcohols,1 phenol,1 ketone and 1 sulfur compound.The standard curve of flavor compounds in Daqu had good linearity,the correlation coefficient(R2)was all above 0.99,the relative standard deviation(RSD)of precision test result was less than 7.26%,the standard addition recovery rate was 80.25%-119.26%,the detection limit of the method was 0.13-50.17μg/kg,and the quantification limit was 0.44-167.22μg/kg.The method had good precision degree and accuracy,and could meet the requirements for accurate quantitative analysis of flavor compounds in Daqu.

关 键 词：高温大曲 风味物质 液液微萃取 气相色谱-质谱联用 前处理条件 优化 

分 类 号：O657.63[理学—分析化学] TS261.7[理学—化学]