超高效液相色谱-串联质谱法检测麦汁和啤酒中的麦香风味物质

引用本文: 李梅, 杨朝霞, 陈华磊, 郝俊光. 超高效液相色谱-串联质谱法检测麦汁和啤酒中的麦香风味物质[J]. 色谱, 2016, 34(3): 258-262. doi: 10.3724/SP.J.1123.2015.10042 shu

Citation: LI Mei, YANG Zhaoxia, CHEN Hualei, HAO Junguang. Determination of sweet flavor compounds in wort and beer by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2016, 34(3): 258-262. doi: 10.3724/SP.J.1123.2015.10042 shu

超高效液相色谱-串联质谱法检测麦汁和啤酒中的麦香风味物质

1.
啤酒生物发酵工程国家重点实验室, 青岛啤酒股份有限公司, 山东青岛 266100
基金项目:
国家高新技术研究发展("863"计划)项目(2013AA102109) ("863"计划)项目(2013AA102109)

青岛创业创新领军人才计划项目(13-cx-15). (13-cx-15)

摘要: 应用超高效液相色谱-串联质谱(UPLC-MS/MS)技术定量检测了啤酒和麦汁中的2,5-二甲基-4-羟基-3(2H)-呋喃酮(DMHF)、2(或5)-乙基-5(或2)-甲基-4-羟基-3(2H)-呋喃酮(EMHF)和2-乙酰吡咯(2-AP)3种麦香风味物质。使用C₁₈固相萃取柱净化样品。采用ACQUITY UPLC HSS T3色谱柱(50 mm×2.1 mm, 1.8 μm)分离,以0.1%(v/v)甲酸水溶液和0.01%(v/v)甲酸乙腈溶液为流动相进行梯度洗脱。结合这3种化合物的保留时间,在正离子模式下,采用多反应监测(MRM)技术进行定量检测。当质量浓度低于1000 μ g/L时,校准曲线的线性良好(R²>0.999)。方法的加标回收率在74.3%~86.7%之间,相对标准偏差(RSD,n=6)在4.8%~7.3%之间。由于酵母发酵时会生成DMHF和EMHF,导致啤酒中这两种物质的含量明显高于麦汁。某些品类啤酒如印度淡色爱尔啤酒(IPA),通常含有较高的麦香风味物质。该法样品处理简单,选择性好,且灵敏、准确、重现性好,可用于啤酒生产的过程控制。

关键词:

English

Determination of sweet flavor compounds in wort and beer by ultra-high performance liquid chromatography-tandem mass spectrometry

1.
State Key Laboratory of Biological Fermentation Engineering of Beer, Tsingtao Brewery Co. Ltd., Qingdao 266100, China
Received Date: 28 October 2015
Fund Project:
国家高新技术研究发展("863"计划)项目(2013AA102109)

青岛创业创新领军人才计划项目(13-cx-15).

Abstract: An ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method was developed for the simultaneous determination of three sweet flavor compounds in wort and beer including 2,5-dimethyl-4-hydroxy-3(2H)-furanone (DMHF), 2(or 5)-ethyl-5(or 2)-methyl-4-hydroxy-3(2H)-furanone (EMHF) and 2-acetylpyrrole (2-AP). C₁₈solid-phase extraction (SPE) tubes were used to clean up samples. The analysis was performed on an ACQUITY UPLC HSS T3 column (50 mm×2.1 mm, 1.8 μm) with gradient elution of mobile phase A (water containing 0.1%(v/v) formic acid) and mobile phase B (acetonitrile containing 0.01%(v/v) formic acid). These three compounds were identified by retention times in positive mode with multiple reaction monitoring (MRM) mode. Good linearities were observed (R²>0.999) in the concentrations less than 1000 μ g/L. The recoveries were in the range of 74.3%-86.7%. The relative standard deviations (RSDs) (n=6) were between 4.8% and 7.3%. Both DMHF and EMHF can be produced by yeast during fermentation, which resulted in apparently higher concentrations in beer than the relevant wort. The concentrations of these compounds may be much higher in certain beer, such as the India Pale (IPA) beer. The method with simple and selective pretreatment measures was sensitive, accurate and reproducible. It may be applied for the quality control in breweries.

Key words:

ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS)
/ furanone
/ 2-acetylpyrrole
/ beer
/ wort

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

超高效液相色谱-串联质谱法检测麦汁和啤酒中的麦香风味物质

English

Determination of sweet flavor compounds in wort and beer by ultra-high performance liquid chromatography-tandem mass spectrometry

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

超高效液相色谱-串联质谱法检测麦汁和啤酒中的麦香风味物质

English

Determination of sweet flavor compounds in wort and beer by ultra-high performance liquid chromatography-tandem mass spectrometry

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

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