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建立了淀粉类食品中丙烯酰胺的QuEChERS前处理结合高效液相色谱-质谱的检测方法。淀粉类食品样品经过2次正己烷脱脂,水和乙腈涡旋振动提取,采取N-丙基乙二胺(PSA)净化方式,以甲醇-水(1:9,v/v)为流动相,Venusil C_(18) MP色谱柱分离,质谱电喷雾电离方式,同位素内标标准曲线法,特定质荷比m/z为72和75定量分析丙烯酰胺及内标。结果表明,丙酰酰胺的定性检出限为3.5μg/kg,定量检出限为12μg/kg,线性定量范围(0.01~2.00)μg/mL,线性相关系数(R~2)为0.9999,加标回收率在90.5%~97.9%范围,相对标准偏差小于3.0%。方法具有操作简单、快速、可靠和较低检测限等优点,成功应用于淀粉类食品中丙烯酰胺含量的检测。
A method for the determination of acrylamide in starchy food by QuEChERS pretreatment combined with high performance liquid chromatography-mass spectrometry was established. Starch samples were extracted with n-hexane, vortexed with water and acetonitrile, and purified by PSA with methanol-water (1: 9, v / v) Venusil C 18 MP column separation, mass spectrometry electrospray ionization, isotope internal standard curve method, specific mass-to-charge ratio m / z 72 and 75 quantitative analysis of acrylamide and internal standard. The results showed that the limit of detection (LOD) of propionamide was 3.5 μg / kg, the limit of quantification was 12 μg / kg, the linear range was 0.01-2.00 μg / mL and the linear correlation coefficient was 0.9999 The standard recoveries ranged from 90.5% to 97.9% with relative standard deviations less than 3.0%. The method has the advantages of simple operation, fast, reliable and lower detection limit, and has been successfully applied to the detection of acrylamide in starchy foods.