高效液相色谱-串联质谱法同时测定食醋中4-甲基咪唑和2-乙酰基-4-(1,2,3,4-四羟基丁基)咪唑  

Simultaneous Determination of 4-Methylimidazole and 2-Acetyl-4-(1,2,3,4-tetrahydroxybutyl)Imidazole in Vinegar by High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：荣维广[1] 宋宁慧[2] 彭凡立[3] 王春蕾[3] 朱峰[1] 阮丽萍[1] 刘华良[1] 吉文亮[1] 

机构地区：[1]江苏省疾病预防控制中心,江苏南京210009 [2]环境保护部南京环境科学研究所,江苏南京210042 [3]东南大学公共卫生学院,江苏南京210009

出　　处：《分析科学学报》2016年第2期223-228,共6页Journal of Analytical Science

基　　金：国家自然科学基金(No.41101307);江苏省科技厅科技支撑计划(No.BE2010745);江苏省"十二五"科教兴卫工程(No.ZX201109)

摘　　要：建立了高效液相色谱-串联质谱法同时检测食醋中4-甲基咪唑（4-Methylimidazole,4-MEI）和2-乙酰基-4-（1,2,3,4-四羟基丁基）咪唑（2-Acetyl-4-（1,2,3,4-tetrahydroxybutyl）imidazole,THI）的方法。样品经超纯水稀释,用氨水溶液调节pH=9.0,采用0.22μm水系微孔滤膜过滤,以乙腈和0.05%氨水为流动相,流速为0.4mL/min,用反相色谱柱Polaris C18-A（150×4.6 mm,3μm）进行分离,采用电喷雾正离子（ESI＋）模式电离,多反应监测（MRM）模式检测,以d6-4-甲基咪唑（d6-4-methylimidazole,d6-4-MEI）作为内标进行定量。4-MEI和THI在0.01-1.0mg/L之间线性关系良好（r〉0.9996）,4-MEI和THI在所有醋中0.2mg/L、0.5mg/L和2.0mg/L三个添加浓度的回收率范围为80.2%-101.4%,相对标准偏差均小于6.4%,浅色的白醋和米醋的检出限为0.06 mg/L,定量限为0.2 mg/L;深色的香醋和陈醋的检出限为0.15mg/L,定量限为0.5mg/L。An analytical method was developed to determine 4-methylimidazole（4-MEI）and 2-acetyl-4-（1,2,3,4-tetrahydroxybutyl）imidazole（THI）in vinegar by high performance liquid chromatographic-electrospray ionization tandem mass spectrometry（HPLC-ESI-MS/MS）.Vinegars were dissolved in Milli-Q water,with the pH value being adjusted to 9.0with ammonium hydroxide,and then filtered through 0.22μm microporous membrane.Then the solution was separated by HPLC system with column Polaris C18-A（150mm×4.6mm,3μm）.The flow rate was 0.4mL/min with a mobile phase consisting of acetonitrile（solvent A）and 0.05%ammonia in water（solvent B）.4-MEI and THI were determined in the mode of electrospray positive ionization（ESI＋）and multiple reaction monitoring（MRM）.d6-4-methylimidazole（d6-4-MEI）was used as the internal standard for the quantitative determination.The method showed good linearity within the concentration range of0.01-1.0 mg/L with the correlation coefficients greater than 0.9996.Recoveries of 4-MEI and THI were between 80.2%-101.4%and relative standard deviations were less than 6.4%at three spiked level of 0.2mg/L,0.5mg/L and 2.0mg/L.The limits of detection（LOD）in white vinegar,rice vinegar,aromatic vinegar and aged vinegar were 0.06mg/L,0.06mg/L,0.15mg/L and 0.15mg/L and the limits of quantitation（LOQ）were 0.2mg/L,0.2mg/L,0.5mg/L and 0.5mg/L,respectively.

关 键 词：高效液相色谱-串联质谱法 4-甲基咪唑 2-乙酰基-4-(1 2 3 4-四羟基丁基)咪唑 食醋 

分 类 号：O657.63[理学—分析化学]