同位素稀释-液液萃取-LC-MS/MS快速测定焙烤食品中丙烯酰胺

Fast Determination of Acrylamide in Baked Foods by Isotope Dilution-Liquid-Liquid Extraction LC-MS/MS

建立了基于同位素稀释-液液萃取-液相色谱-串联质谱法快速测定焙烤食品中丙烯酰胺含量的分析方法。样品经同位素稀释,超纯水提取,乙酸乙酯净化,经HSS T3色谱柱分离,以0.1%甲酸水-甲醇为流动相,梯度洗脱,串联质谱多反应监测正离子扫描,内标法定量。结果显示,在2.5~400μg/L范围内,相关系数大于0.999,方法定量限为5μg/kg,平均回收率为95.6%~105%,平均相对标准偏差为3.7%~8.9%。本方法操作简便、准确性及适用性良好、成本较低,适用于大批量焙烤食品中丙烯酰胺的快速测定。

A method for the determination of acrylamide in baked foods using liquid-liquid extraction-stable isotope dilution liquid chromatography-tandem mass spectrometry was established.The samples were processed by isotope dilution,extracted by water and purified by ethyl acetate,and then separated by HSS T3 column using gradient elution with 0.1%formic acid solution and acetonitrile as mobile phases.Acrylamide was detected by tandem mass spectrometry in the multi-reaction monitoring mode with positive electrospray ionization and quantified by internal standard method.The results showed that the coefficient of correlation was larger than 0.999 within the range of 2.5~400μg/L.The quantitation limit of the method was 5μg/kg and the mean recovery ranged from 95.6%to 105%with the mean relative standard deviation(RSD)ranged from 3.7%to 8.9%.The established method is simple,accurate,suitable and low cost for the fast determination of acrylamide in large quantities of baked foods.