液相色谱-电喷雾质谱/质谱法测定高温烹制的淀粉类食品中的丙烯酰胺

以C18反相色谱柱为分析柱,以0.1%甲酸水溶液-甲醇(体积比为98∶2)为流动相,采用同位素稀释液相色谱-电喷雾 质谱/质谱(LC-MS/MS)技术对加热淀粉类食品中的丙烯酰胺进行了测定。利用Oasis HLB固相萃取柱对样品进行净化。方 法的线性范围为10～500 μg/L,线性相关系数为0.9995。方法的定性检出限为6 μg/kg,定量检出限为20 μg/kg。高 、中、低3个浓度水平的加标回收率为96.8%~97.4%,相对标准偏差小于10%。

Determination of Acrylamide in Heated Starchy Food by Liquid Chromatography-Electrospray Ionization

An isotope dilution liquid chromatographic-electrospray ionization tandem mass spectrometric method has been established for the determination of acrylamide in heated starchy food with a C18 analytical column and methanol-water containing 0.1% formic acid (2:98, v/v) as mobile phases. The clean-up of samples was performed on an Oasis HLB solid phase extraction cartridge. The calibration curve of acrylamide showed good linearity in the range of 10-500 microg/L with correlation coefficient of 0.9995. The detection limit of the method was 6 microg/kg (S/N = 3), and the limit of quantification was 20 microg/kg (S/N = 10). The average recoveries at three levels ranged from 96.8% to 97.4% (n = 5), and the relative standard derivations were lower than 10%.