SPE-GC-MS/MS法同时检测贵州酱香型白酒中12种吡嗪类化合物  

Simultaneous detection of 12 pyrazines in Guizhou sauce-flavor Baijiu by SPE-GC-MS/MS

作　　者：杨金川 黄家岭 白雪梅 张吉敏 YANG Jinchuan;HANG Jialing;BAI Xuemei;ZHANG Jimin(Guizhou Institute of Products Quality Inspection&Testing,Guiyang 550001,China;Guizhou Advertising Monitoring Center,Guiyang 550001,China)

机构地区：[1]贵州省产品质量检验检测院,贵州贵阳550001 [2]贵州省广告监测中心,贵州贵阳550001

出　　处：《中国酿造》2025年第2期261-267,共7页China Brewing

基　　金：贵州省产品质量检验检测院科研项目[院科(2022)005号]。

摘　　要：该研究建立了一种固相萃取(SPE)前处理结合气相色谱-串联质谱(GC-MS/MS)检测贵州酱香型白酒中12种吡嗪类化合物含量的方法。样品经碱性硅藻土固相萃取柱净化浓缩后,采用GC-MS/MS选择监测模式(SRM)测定,以内标法定量。结果表明,12种吡嗪类化合物在5~2000μg/L含量范围内呈良好线性关系,相关系数(R2)均>0.99,方法的检出限(LOD)为0.18~2.52μg/L,定量限(LOQ)为0.59~8.39μg/L。12种吡嗪类化合物的平均加标回收率在85.5%~105.0%,精密度实验结果相对标准偏差(RSD)在4.80%~9.70%。市售贵州7种酱香型白酒检出12种吡嗪类化合物,总含量为3.84~8.48 mg/L,不同酱香型白酒中各吡嗪化合物的含量不同,但其中四甲基吡嗪和三甲基吡嗪类含量最高,分别为1.00~3.91 mg/L和0.68~1.79 mg/L。该方法操作简单、灵敏度高,准确度及精密度良好,能够对酱香型白酒中吡嗪类化合物进行快速检测。A method was established for the simultaneous determination of 12 pyrazines in Guizhou sauce-flavor(Jiangxiangxing)Baijiu by solid phase extraction(SPE)pretreatment combined with gas chromatography-tandem mass spectrometry(GC-MS/MS).The samples were purified and concentrated by alkaline diatomite solid-phase extraction column,then determined by GC-MS/MS selective monitoring mode(SRM)and quantified by internal standard method.The results showed that there was a good linear relationship between the contents of 12 pyrazine in the range of 5-2000μg/L,and the correlation coefficients(R2)were all over 0.99.The limit of detection(LOD)were 0.18-2.52μg/L,and limit of quantitative(LOQ)were 0.59-8.39μg/L.The average recoveries rates of 12 pyrazines were 85.5%-105.0%,and the relative standard deviations(RSD)of precision experiments were 4.80%-9.70%.12 kinds of pyrazines were detected in 7 kinds of sauce-flavor Baijiu in Guizhou,with a total content of 3.84-8.48 mg/L.The contents of each pyrazine in different sauce-flavor Baijiu were different,but the contents of tetramethylpyrazine and trimethylpyrazine were the highest,which were 1.00-3.91 mg/L and 0.68-1.79 mg/L,respectively.The method had the advantages of simple operation,high sensitivity,good accuracy and precision,and could be used for rapid detection of pyrazines in sauce-flavor Baijiu.

关 键 词：固相萃取 气相色谱-串联质谱 酱香型白酒 吡嗪类化合物 同时检测 

分 类 号：TS261.2[轻工技术与工程—发酵工程]