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气相色谱质谱联用法测定封窖泥中的两种土霉味物质
引用本文:黄箭,谢正敏,施思,魏金萍,张倩,范涛,薛润萍.气相色谱质谱联用法测定封窖泥中的两种土霉味物质[J].中国酿造,2023,42(2):215-220.
作者姓名:黄箭  谢正敏  施思  魏金萍  张倩  范涛  薛润萍
作者单位:(宜宾五粮液股份有限公司 中国轻工业浓香型白酒固态发酵重点实验室,四川 宜宾 644000)
基金项目:宜宾市科技计划项目(2020NY001);
摘    要:土臭素(GSM)和二甲基异茨醇(2-MIB)是引起白酒土霉味的主要物质。该研究建立了顶空固相微萃取(HS-SPME)结合气相色谱-质谱联用(GC-MS)法测定封窖泥中GSM和2-MIB。该实验对比常压蒸馏萃取和超声波提取对封窖泥中GSM和2-MIB的提取效果,优化顶空固相微萃取(HS-SPME)条件,并对HS-SPME和直接进样两种模式检测结果进行比较。结果表明,超声波提取的最佳条件为:10 m L体积分数50%的乙醇提取两次;HS-SPME最佳萃取条件为:采用65μm PDMS/DVB萃取头,萃取温度50℃,NaCl添加量0.3 g/m L,萃取时间50 min,体积分数5%乙醇提取两次。HS-SPME和直接进样两种进样模式检测结果相对标准偏差(RSD)在3.9%~12.9%之间,相关系数(R2)均≥0.997,加标回收率均在78.47%~110.24%。该方法操作简便高效,精密度、准确度高,适用于封窖泥中GSM和2-MIB的检测。

关 键 词:顶空固相微萃取  气相色谱质谱联用法  土臭素  二甲基异茨醇  封窖泥

Determination of two musty-smelling compounds in pit-sealing mud by GC-MS
HUANG Jian,XIE Zhengmin,SHI Si,WEI Jinping,ZHANG Qian,FAN Tao,XUE Runping.Determination of two musty-smelling compounds in pit-sealing mud by GC-MS[J].China Brewing,2023,42(2):215-220.
Authors:HUANG Jian  XIE Zhengmin  SHI Si  WEI Jinping  ZHANG Qian  FAN Tao  XUE Runping
Affiliation:(Key Laboratory of Wuliangye-Flavor Liquor Solid-State Fermentation, China National Light Industry, Yibin Wuliangye Co., Ltd., Yibin 644000, China)
Abstract:Geosmin (GSM) and 2-methylisoborneol (2-MIB) are the main substances causing musty smell of Baijiu. In this study, headspace solid-phase microextraction (HS-SPME) combined with GC-MS was established for the determination of GSM and 2-MIB in pit-sealing mud. The extraction effects of atmospheric distillation extraction and ultrasonic extraction on GSM and 2-MIB in pit-sealing mud were compared in this experiment, HS-SPME conditions were optimized, and the determination results of two modes of HS-SPME and direct injection were compared. The results showed that the optimal conditions for ultrasonic extraction were as follows: extraction twice with 10 ml of volume fraction 50% ethanol. The optimal extraction conditions for HS-SPME were as follows: 65 μm PDMS/DVB extraction head, extraction temperature 50 ℃, NaCl addition 0.3 g/ml, time 50 min, and extraction twice with volume fraction 50% ethanol. The relative standard deviation (RSD) of the detection results of the two injection modes of HS-SPME and direct injection were 3.9%-12.9%, the correlation coefficient (R2)≥0.997, and the standard recovery rates were 78.47%-110.24%. The method was simple and efficient with high precision and accuracy, and was suitable for the detection of GSM and 2-MIB in pit-sealing mud.
Keywords:headspace solid-phase microextraction  GC-MS  geosmin  2-methylisoborneol  pit-sealing mud  
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