固相萃取-液相色谱-串联质谱法测定市售卤肉制品中5种杂环胺含量

Determination of 5 Kinds of Heterocyclic Amines in Stewed Meat Using Solid Phase Extraction and Liquid Chromatography-tandem Mass Spectrometry

建立了LC-MS/MS快速检测卤肉制品中MeIQ、MeIQx、4,8-DiMeIQx、7,8-DiMeIQx和PhIP 5种杂环胺的方法。样品经40 g/L NaOH-甲醇溶液超声提取,用聚苯乙烯二乙烯苯固相萃取小柱(Poly-Sery PSD)净化,在电喷雾离子源正离子(ESI^+)多反应监测(MRM)模式下进行测定。5种杂环胺化合物在0.1~10μg/L范围内线性关系良好,决定系数R^2在0.9976~0.9997之间,在空白样品中的平均添加回收率为76.9%~127.7%,日内相对标准偏差(RSD)为1.0%~9.5%,日间相对标准偏差(RSD)为2.1%~8.7%。在信噪比(S/N)分别为3和10时各化合物的LODs在0.01~0.1μg/kg,LOQs在0.025~0.25μg/kg。该方法分析时间短,准确度高,精密度好,可满足卤肉中多种杂环胺同时检测的要求。

A rapid LC-MS/MS method for the determination of 5 kinds of heterocyclic amines(MeIQ,MeIQx,4,8-DiMeIQx,7,8-DiMeIQx and PhIP)in stewed meat products were established. The samples were extracted by ultrasonic extraction with 40 g/L NaOH-methanol solution and purified by polystyrene divinylbenzene solid phase extraction column(Poly-Sery PSD). The electrospray ion source positive ion(ESI^+)and multi-reaction monitoring(MRM)mode were used for the determination of the 5 kinds of heterocyclic amines. The calibration curves of the 5 kinds of heterocyclic amines showed a good linear relationship in the ranges of 0.1~10 μg/L and the decisive coefficients(R^2)were in the range of 0.9976~0.9997.The average recoveries of spikes samples ranged from 76.9% to 127.7% with relative standard deviations(RSD)of intra-and inter-day in the ranges of 1.0%~9.5% and 2.1%~8.7%,respectively. The limits of detection(LODs)and quantification(LOQs)were 0.01~0.1 and 0.025~0.25 μg/kg,respectively. The method has the advantages of short analysis time,high accuracy and good precision,and can meet the requirements of simultaneous detection of various heterocyclic amines in stewed meat.