液相色谱-串联质谱测定葡萄酒中4-乙基苯酚和4-乙基愈创木酚

Determination of 4-ethylphenol and 4-ethylguaiacol in wine by liquid chromatography-tandem mass spectrometry

目的建立液相色谱-串联质谱法同时测定葡萄酒中4-乙基苯酚和4-乙基愈创木酚的方法。方法样品经甲醇(1.0%甲酸)溶液提取,Oasis HLB固相萃取柱净化后,采用液相色谱-串联质谱法负离子模式检测,通过多反应监测模式,对葡萄酒中4-乙基苯酚和4-乙基愈创木酚进行定量分析。结果 4-乙基苯酚和4-乙基愈创木酚线性范围为0.01～0.1μg/m L,定量限(limit of quantification,LOQ)为0.01μg/kg,加标回收率为77.6%～93.5%,相对标准偏差均小于10%。结论本方法操作简单,结果准确可靠,对葡萄酒中4-乙基苯酚和4-乙基愈创木酚的检测具有较强的适用性。

Objective To establish a method for determination of 4-ethylphenol and 4-ethylguaiacol in wine by liquid chromatography-tandem mass spectrometry（LC-MS/MS）. Methods The samples were extracted with methyl alcohol（1% formic acid）, and then purified by the Oasis HLB SPE column. Finally the 4-ethylphenol and 4-ethylguaiacol in wine were measured by LC-MS/MS using multiple reaction monitoring（MRM） with negative ion mode. Results The 4-ethylphenol and 4-ethylguaiacol showed a good linear relationship in the concentration range of 0.01-0.1 μg/m L, the limit of quantification（LOQ） was 0.01 μg/kg, the average recoveries were 77.6%-93.5%, and the relative standard deviation（RSD） was not more than 10%. Conclusion This method is simple and accurate, which is suitable for determination of 4-ethylphenol and 4-ethylguaiacol in wine.which is suitable for determination of 4-ethylphenol and 4-ethylguaiacol in wine.