高效液相色谱-串联质谱联用测定富含淀粉食品中丙烯酰胺

Determination of Acrylamiade in Cooked Starch-enriched Food by High Performance Liquid Chromatography Tandem Mass Spectrometry

以甲基阿烯酰胺作为内标物，用高效液相色谱／串联质谱（HPLC／MS／MS）法测定食品中的丙烯酰胺。均质后的食品样品，加入正己烷经液-液分配去除脂肪，用蒸馏水提取丙烯酰胺，Carrez试剂净化提取样品，净化液经离心后过0．45μm微孔滤膜，采用HPLC／MS／MS电喷雾电离（ESI），阳离子，多反应监测（MRM）模式检测，外标法定量。方法的线性范围为2～500μg／L，线性相关系数为0．9997，检出限为2μg／kg；高中低3个水平的加标回收率分别为99．4％、99．6％和98．4％；相对标准偏差（RSD）均小于7．8％。

With the aid of methyl-acrylamide internal standard, a high performance liquid chromatography tandem mass spectrometric method was established for the determination of acrylamide in food. Homogenized food samples were first defatted by liquid-liquid partition, and extracted with distilled water. Then cleaned by Carrez solution and centrifuged. Identification was achieved by electrospray ionization （ESI） in positive mode using multiple reaction monitoring. The calibration curve of acrylamide showed good linearity in the range of 2～500 mg/L with correlation coefficient of 0.9997. The detection limit of the method was 2 μg/kg （S/N = 3）. The spiked at three levels ranged from 98.4% to 99.6% （n = 6） and the relative standard derivations were lower than 7.8%.