顶空-气相色谱串联质谱法测定白酒和葡萄酒中甲醇的含量

Determination of Methanol in Baijiu and Wine by Headspace-gas Chromatography Tandem Mass Spectrometry

赵四标 ¹马艳红 ¹刁玉华 ¹万静 ¹王灿 ¹陈娴¹

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作者信息

1. 昆明市食品药品检验所食品检验中心,云南昆明 650010
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摘要

利用顶空-气相色谱串联质谱(HS-GC/MSMS)技术,建立白酒和葡萄酒中甲醇定性定量的检测方法.样品无需前处理直接装入顶空瓶中自动完成进样,顶空平衡温度为80.0 ℃,恒温时间35 min,盐析剂为2 g氯化钠,采用分流进样,分流比为100∶1,以电子轰击源(EI)为离子源,采用多反应监测(MRM)模式进行分析.经确认,白酒采用内标法、葡萄酒采用外标法得到的准确度更高.甲醇在0.201416～10.0708 mg/L和10.0708～402.832 mg/L的质量浓度范围内线性关系良好,相关系数R2均＞0.999,方法测定低限为0.2 mg/L,加标回收率为97.51％～102.05％,精密度RSD为0.583％～3.814％(n=6).方法简便、灵敏度高、干扰少、准确度高,适合于白酒和葡萄酒中甲醇的快速检测.

Abstract

To establish qualitative and quantitative method for the determination of methanol in Baijiu and wine by headspace-gas chromatogra-phy tandem mass spectrometry(HS-GC/MSMS).The sample is directly loaded into a headspace bottle without pre-treatment and automati-cally injected.The headspace equilibrium temperature is 80.0 ℃,the constant temperature time is 35 minutes,the salting-out agent is 2 g NaCl.It uses split injection with a split ratio of 100∶1,uses an electron impact source(EI)as the ion source,and uses multiple response monito-ring(MRM)mode for analysis.It is confirmed that the accuracy of internal standard method for Baijiu and external standard method for wine is higher.The linear relationship of methanol has good in the range of 0.201416～10.0708 mg/L and 10.0708～402.832 mg/L,with correlation coefficient R2 greater than 0.999,the recovery rate is 97.51％～102.05％,and the precision RSD is 0.583％～3.814％(n=6).This method is simple,sensitive,less interference,high accuracy,suitable for rapid detection of methanol in Baijiu and wine.

关键词

甲醇/白酒/葡萄酒/顶空-气相色谱串联质谱/多反应监测

Key words

Methanol/Baijiu/Wine/Headspace-Gas Chromatography Tandem Mass Spectrometry/Multiple Response Monitoring

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出版年

2024

云南化工

云南省化工研究院云天化集团有限责任公司云南煤化工集团有限公司云南省化学化工学会

云南化工

影响因子：0.272

ISSN：1004-275X

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