UPLC-MS/MS同时测定不同年份酱香型白酒中12种吡嗪类化合物  

Simultaneous determination of 12 pyrazine compounds in sauce-flavor Baijiu of different aging years by UPLC-MS/MS

作　　者：杨沙 罗玉航 张季 侯睿 YANG Sha;LUO Yuhang;ZHANG Ji;HOU Rui(Zunyi Institute of Products Quality Inspection and Testing,Zunyi 563099,China)

机构地区：[1]遵义市产品质量检验检测院,贵州遵义563099

出　　处：《中国酿造》2024年第10期250-257,共8页China Brewing

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：建立了超高效液相色谱串联质谱(UPLC-MS/MS)技术同时测定不同年份的酱香型白酒中12种吡嗪类化合物的分析方法。结果表明,12种吡嗪类化合物在质量浓度50~1000μg/L范围内线性关系良好,相关系数(R2)均>0.99,检出限在0.051~6.00μg/L,定量限在0.18~21.42μg/L,日内精密度试验结果相对标准偏差(RSD)为0.67%~2.72%,在0.1μg/m L、0.2μg/m L、0.5μg/m L 3个质量浓度水平下的加标回收率为80.6%~108.7%。12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,在15年酱香型白酒中含量达到最高值。通过多元统计分析找到不同年份酱香型白酒的特征差异性化合物,分别为2,3,5,6-四甲基吡嗪、2,6-二甲基吡嗪和2,3-二甲基吡嗪,这些特征差异性化合物可能为主要差异性指标成分,可以用于区分不同年份的酱香型白酒。该方法前处理简单、分析时间短、稳定性高,为酱香型白酒中吡嗪类化合物的检测提供了相关技术依据。A analysis method for simultaneous determination of 12 pyrazine compounds in sauce-flavor(Jiangxiangxing)Baijiu samples of different aging years by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The results showed that 12 pyrazine compounds had a good linearity in the range of 50-1000μg/L(R2>0.99).The limits of detection were 0.051-6.00μg/L,and the limits of quantitation were 0.18-21.42μg/L.The relative standard deviation(RSD)of intra-day precision tests results was 0.67%-2.72%.At different mass concentrations of 0.1,0.2 and 0.5μg/ml,the standard recovery rates were 80.6%-108.7%.The contents of the 12 pyrazine compounds showed an increasing trend with the increase of the aging year of sauce-flavor Baijiu samples,and reached the highest value in the 15-year-old sauce-flavor Baijiu samples.Through multivariate statistical analysis,the characteristic differential compounds of sauce-flavor Baijiu samples of different aging years were found,which were 2,3,5,6-tetramethylpyrazine,2,6-dimethylpyrazine and 2,3-dimethylpyrazine,respectively.These characteristic difference compounds might be the main difference index components,which could be used to distinguish sauce-flavor Baijiu of different aging years.The method had the advantages of simple pretreatment,short analysis time and high stability,and provided relevant technical basis for the detection of pyrazine compounds in sauce-flavorBaijiu samples.

关 键 词：酱香型白酒 吡嗪类化合物 年份酒 超高效液相色谱-串联质谱法 

分 类 号：TS262.3[轻工技术与工程—发酵工程] O657.63[轻工技术与工程—食品科学与工程]