建立了超高压液相色谱-串联质谱法（UHPLC-MS/MS）测定速溶咖啡和曲奇饼干中丙烯酰胺含量的方法。分别称取速溶咖啡或曲奇饼干样品2.0 g，用乙腈提取2次（10 mL×2），正己烷除脂2次（10 mL×2），取10 mL乙腈相于40℃减压浓缩至近干，加水1 mL溶解，经0.45 μm水系滤膜过滤，得待测液。以Aglient Eclipse Plus C₁₈色谱柱为固定相，以5%（体积分数）甲醇溶液为流动相，在流量0.15 mL·min^-1下进行等度洗脱，电喷雾正离子（ESI⁺）模式和多反应监测（MRM）模式下测定，内标法定量。结果显示：丙烯酰胺标准曲线的线性范围为0.005~1.00 mg·L^-1，检出限（3S/N）为0.000 3 mg·L^-1；对速溶咖啡和曲奇饼干样品进行3个浓度水平的加标回收试验，回收率为88.9%~111%，测定值的相对标准偏差（n=5）为2.5%~14%。

A method for the determination of acrylamide in instant coffee and cookies by UHPLC-MS/MS was developed. Instant coffee or cookies samples of 2.0 g was extracted twice with acetonitrile (10 mL×2) and degreased twice with hexane (10 mL×2). Acetonitrile phase of 10 mL was concentrated to nearly dryness under reducing pressure at 40 ℃. Water of 1 mL was added to the residue, and the solution obtained was filtered by 0.45 μm water filtration membrane. Aglient EclipsePlus C₁₈ column was used as stationary phase, and 5% (φ) methanol solution at a flow rate of 0.15 mL·min^-1 was used as mobile phase for isocratic elution. Acrylamide was detected by ESI⁺ and MRM mode, and quantified by internal standard method. As shown by the results, linear range of the standard curve of acrylamide was 0.005-1.00 mg·L^-1, with detection limit (3S/N) of 0.000 3 mg·L^-1. Recovery test was made on the instant coffee and cookies samples at 3 concentration levels by standard addition method, giving results in the range of 88.9%-111%, with RSDs (n=5) of the determined values ranged from 2.5% to 14%.