加速溶剂萃取-液相色谱-离子阱飞行时间质谱法同时测定烹调食品中丙烯酰胺和3种杂环胺

Simultaneous Determination of Acrylamide and 3 Heterocyclic Amines in Cooked Food by LC-IT-TOF-MS with Accelerated Solvent Extraction

提出了用加速溶剂萃取-液相色谱-离子阱飞行时间质谱法测定烹调食品中丙烯酰胺和3种常见杂环胺的含量。样品经乙腈提取，40℃水浴中氮吹至干，残留物用30mmol·L^-1甲酸-乙腈（9＋1）混合液定容，经Alltima C18色谱柱分离，以不同体积比的30mmol·L^-1甲酸溶液和乙腈的混合液为流动相梯度洗脱，采用正离子模式监测。丙烯酰胺和3种杂环胺的质量浓度分别在0．1～5．0mg·L^-1和0．002-1．0mg·L^-1范围内与其峰面积呈线性关系，检出限（3s／N）分别为10，0．3～0．9μg·kg^-1。以实样为基体，采用标准加入法做回收试验，测得回收率在79．5％～105％之间，测定值的相对标准偏差（n=6）在2．1％～6．9％之间。

A method for simultaneous determination of acrylamide and 3 heterocyclic amines in cooked food by LC-IT-TOF-MS with ASE was proposed. The samples were extracted with acetonitrile, and the extract was evaporated to dryness at 40℃ with N2-blowing. The residues were dissolved with a mixture of 30 mmol ·L^-1. formic acid solfl, and acetonitrile （9 ＋1） and used for LC-IT-TOF-MS analysis. Alhima C18 column was used as stationary phase, and mixtures of 30 mmol · L^-1 formic acid soln, and acetonitrile of different ratio were used as mobile phase in gradient elution; positive electrospray ionization was used in the detection. Linear relationships between values of peak area and mass concentration of acrylamide and the 3 heterocyelic amines were kept in the ranges of 0. 1-5.0 mg· L^-1 and 0. 002-1.0 mg · L ^-1 respectively, with detection limits （3S/N） of 10μg ·kg^-1 for acrylamide and in the range of 0.3-0.9μg · kg ^-1 （for the 3 heferocyclic amines）. Recovery were tested by the standard addition method, giving values of recovery in the range of 79.5%-105% with RSD＇s （n = 6） in the range of 2. 1%-6.9%.