液相色谱-离子阱-飞行时间串联质谱同时检测葡萄酒中14种杂环胺

Determination of 14 heterocyclic aromatic amines in wine by liquid chromatography-ion trap-time of flight tandem mass spectrometry

建立了液相色谱-离子阱-飞行时间串联质谱法(LC-IT-TOF MS)同时测定葡萄酒中14种杂环胺(HAAs)残留量的分析方法。样品于乙酸乙酯碱性条件下提取,内标法定量,Phenomenex Kinetex C18100A色谱柱(100 mm×2.1mm,2.6μm)分离,以乙腈和30 mmol/L甲酸铵为流动相进行梯度洗脱。实验结果表明,2-氨基-3,7,8-三甲基咪唑[4,5-f]喹喔啉在1～500μg/L、2-氨基-3,8-二甲基咪唑[4,5-f]喹喔啉在10～500μg/L、其他12种杂环胺在5～500μg/L质量浓度范围内线性良好,相关系数均不小于0.994 5,检出限(以信噪比为3计)0.33～1.77μg/L。14种杂环胺在加标水平为10、50、100μg/L时的回收率分别为71.6%～96.4%、72.9%～101.9%、74.5%～103.3%,相对标准偏差(RSD,n=6)分别为2.9%～7.9%、1.7%～5.3%、1.8%～4.8%。结果显示该方法线性范围宽,精密度和准确度较高,分析时间短,净化效果好,可满足葡萄酒中多种杂环胺残留同时检测的要求。

A rapid qualitative and quantitative analytical method was developed for the simultaneous determination of 14 heterocyclic aromatic amines（HAAs） in wine by liquid chromatography-ion trap-time of flight tandem mass spectrometry（LC-IT-TOF MS）.HAAs were extracted from the samples by ethyl acetate under alkaline condition.The quantitation was carried out using internal standard method.The separation of HAAs was carried out based on Phenomenex Kinetex C18 100A column（100 mm×2.1 mm,2.6 μm）,with a gradient elution of acetonitrile and 30 mmol/L ammonium formate at a flow rate of 0.4 mL/min.The analytes were detected under positive-ion electrospray ionization mode.The results showed that the linear ranges of the 14 HAAs were 1-500 μg/L with limits of detection（signal/noise=3） of 0.33-1.77 μg/L.The average recoveries of all the compounds spiked in wine samples at three levels of 10,50,100 μg/L were in the ranges of 71.6%-96.4%,72.9%-101.9%,74.5%-103.3%,with the corresponding relative standard deviations（RSDs,n=6） of 2.9%-7.9% 、1.7%-5.3% 、1.8%-4.8%,respectively.The established method is simple,rapid,accurate,and has wide linear range and high sensitivity.It can be applied to the simultaneous analysis of the HAAs in wine.