建立了同时测定焙烤食品中丙烯酰胺、4-甲基咪唑和5-羟甲基糠醛的超高效液相色谱-串联质谱（UPLC-MS/MS）分析方法。样品中加入同位素内标后，以水和乙腈超声提取，QuEChERS净化，正己烷脱脂，UPLC-MS/MS分离检测，丙烯酰胺和4-甲基咪唑以同位素内标定量。在优化条件下，3种待测物的方法检出限在1.5 μg/kg~7.0 μg/kg之间；在2.0 μg/L~500 μg/L浓度范围内线性关系良好，相关系数均大于0.9990；在面包、蛋糕和饼干样品中进行3个水平的添加实验，平均回收率（n=6）为87.8~115.7%，日内精密度为3.2~9.6%；日间精密度（n=5）小于11.5%。本方法净化效果好，灵敏度高、准确性好，适用于焙烤食品中丙烯酰胺、4-甲基咪唑和5-羟甲基糠醛的同时测定。

The isotope internal standard was added into the samples, and then the mixture successively underwent supersonic extraction with water and acetonitrile, purification with QuEChERS, degreasing with hexane, and detection with UPLC-MS/MS. Acrylamide and 4-methylimidazole were quantified by isotope internal standard. Under the optimized conditions, the LOD of acrylamide, 4-methylimidazole and 5-hydroxymethylfurfural ranged from 1.5 to 7.0 μg/kg, and the linear range were 2.0~500 μg/L with the correlation coefficients more than 0.9990. The average recoveries ranged from 87.8% to 115.7%, and within-day precisions in a range of 3.2~9.6% when three levels of standard were spiked into bread, cake and biscuits. The inter-day precisions were less than 11.5%. The developed method is characterized by the excellent purification effect, sensitivity and accuracy, and it is competent for the detection of acrylamide, 4-methylimidazole and 5-hydroxymethylfurfural in baking food.

国家自然科学基金项目（21102021）和广东省科技计划项目（2010B10800027）资助