【摘要】 建立了分散固相萃取-超高效液相色谱-串联质谱法测定火锅底料中丙烯酰胺含量。样品经乙腈（含体积分数2%的甲酸）提取、正己烷-石油醚（体积比为1∶1）脱脂后，经吸附剂组合(50 mg MgSO4、150 mg PSA、50 mg C₁₈、15 mg GCB、15 mg SCX)净化，采用HSS T3色谱柱分离，以0.1%甲酸-乙腈为流动相进行梯度洗脱，在ESI⁺-MRM模式下检测，以丙烯酰胺-¹³C₃内标法定量。丙烯酰胺质量浓度在0.5～500 ng/mL内，其质量浓度与内标物质量浓度的比值与二者色谱峰面积的比值线性关系良好，相关系数均不小于0.999 1，检出限和定量限分别为0.05μg/kg和0.2μg/kg。样品加标平均回收率为86.0%～99.6%，测定结果的相对标准偏差为2.3%～6.6%（n=6）。该方法操作简便、重现性好，适用于高脂/辛辣基质中丙烯酰胺的快速准确检测。更多还原

【Abstract】 An analytical method was established for the determination of acrylamide in hot pot base by ultraperformance liquid chromatography-tandem mass spectrometry with dispersive solid-phase extraction. Samples were extracted with acetonitrile containing 2% formic acid, and degreased with n-hexane-petroleum ether（volume ratio of 1:1）, then purified using a composite sorbent consisting of 50 mg MgSO₄, 150 mg PSA, 50 mg C₁₈, 15 mg GCB, and 15 mg SCX. Separation was performed on an HSS T3 column with gradient elution using 0.1% formic acid aqueous solution and acetonitrile as the mobile phase. Detection was carried out in the ESI+-MRM mode, and quantification was achieved by the ¹³C₃-labeled acrylamide internal standard method. The mass concentration of acrylamide was in the range of 0.5 ng/mL-500 ng/mL, and the ratio of its mass concentration to internal standard mass concentration had a good linear relationship with the ratio of their chromatographic peak area, with correlation coefficients all not less than 0.999 1. The limit of detection and limit of quantification were 0.05 μg/kg and 0.2 μg/kg, respectively. The average recoveries from spiked samples ranged from 86.0% to 99.6%, and the relative standard deviations for six parallel determinations were 2.3%-6.6%. This method is simple to operate, exhibits excellent reproducibility, and is well suited for the rapid and accurate determination of acrylamide in high-fat/spicy matrices.更多还原