高效液相色谱法同时测定不同年份酱香型白酒中12种吡嗪化合物含量  

Simultaneous determination of 12 kinds of pyrazine compounds in different vintages of Maotai-flavor Baijiu by high performance liquid chromatography

作　　者：杨沙 罗玉航 张季 侯睿 YANG Sha;LUO Yu-Hang;ZHANG Ji;HOU Rui(Product Quality Inspection and Testing Institute in Zunyi,Zunyi 563099,China)

机构地区：[1]遵义市产品质量检验检测院,遵义563099

出　　处：《食品安全质量检测学报》2024年第12期220-229,共10页Journal of Food Safety and Quality

基　　金：贵州省科技计划项目(黔科合支撑[2023]一般386)、贵州省科技计划项目(黔科合支撑[2023]一般364);国家市场监督管理总局科技计划项目(2022MK117);遵义市科技创新人才团队培养计划项目(遵市科人才[2023]1号)。

摘　　要：目的建立高效液相色谱法(high performance liquid chromatography,HPLC)同时测定不同年份酱香型白酒中12种吡嗪化合物含量的分析方法。方法样品经碱化后用乙醚萃取,浓缩后用甲醇定容。采用C6苯基柱(250 mm×4.6 mm,5.0μm)测定吡嗪类化合物的含量,结合多元统计分析,对不同年份酱香型白酒中吡嗪类化合物进行差异分析。结果12种吡嗪化合物线性表现良好,在质量浓度0.1~10.0μg/mL范围内,相关系数(r^(2))均大于0.99,检出限在0.06~0.29μg/mL,重复性相对标准偏差(relative standard deviations,RSDs)范围均在1.3%~2.8%,在1、2、5μg/mL3个浓度水平下的加标回收率为80.8%~108.3%,精密度RSDs范围均在0.27%~4.80%。11种吡嗪类化合物随着酱香型白酒贮存年份的增加,其含量均呈现上升态势。结论本研究建立了一种灵敏度高、重现性好且适用于不同年份酱香型白酒中12种吡嗪化合物的定量分析方法。该研究表明吡嗪类化合物含量的高低与酱香型白酒储存年份的长短存在一定的关联性。Objective To establish an analysis method for the simultaneous determination of 12 kinds of pyrazine compounds in different vintages of Maotai-flavor Baijiu samples by high performance liquid chromatography(HPLC).Methods The Baijiu samples were extracted with ether after alkalization,concentrated and then fixed with methanol.The content of pyrazine compounds was determined by C6 phenyl column(250 mm×4.6 mm,5.0μm),and the differences of pyrazine compounds in Maotai-flavor Baijiu samples of different vintages was analyzed by multivariate statistical analysis.Results The linear relationship of the 12 kinds of pyrazine compounds was good in the concentration range of 0.1–10.0μg/mL,and the correlation coefficients(r^(2))were all greater than 0.99,and the detection limits were 0.06–0.29μg/mL,with the relative standard deviations(RSDs)of reproducibility were 1.3%–2.8%.At different concentrations of 1,2 and 5μg/mL,the standard recoveries were 80.8%–108.3%,and the RSDs of precision were all in the range of 0.27%~4.80%.The content of the 11 kinds of pyrazine compounds showed an increasing trend with the increase of the storage year of Maotai-flavor Baijiu samples.Conclusion In this study,a high sensitivity and good reproducibility for the quantitative analysis of 12 kinds of pyrazine compounds in Maotai-flavor Baijiu samples of different vintages is established.This study showed that there is a correlation between the content of pyrazine compounds and the storage year of Maotai-flavor Baijiu samples.

关 键 词：酱香型白酒 吡嗪类化合物 年份酒 高效液相色谱法 

分 类 号：TS262.33[轻工技术与工程—发酵工程] O657.72[轻工技术与工程—食品科学与工程]