气相色谱-四极杆-飞行时间质谱仪分析油脂食品中多种邻苯二甲酸酯类化合物残留

摘要

利用气相色谱-四极杆-飞行时间质谱(GC-QTOF MS)技术建立了油脂食品中23种邻苯二甲酸酯类快速检测方法.样品采用乙腈-甲基叔丁基醚(9∶1,v/v)提取,PSA分散剂净化,经GC-QTOF MS测定,采用外标法定量.在全扫描采集模式下,以特征离子峰的峰面积定量,以化合物的保留时间、精确质量数及谱库检索定准确性.23种化合物在线性范围内均呈现良好的线性关系,相关系数均大于0.99,23种化合物的定量限(S/N=1o)为0.05～0.1mg/kg,在0.1～5.0mg/kg 3个添加水平下的平均回收率为79％ ～ 112％,相对标准偏差(RSD,n=6)均低于14％.该方法简便、快速、灵敏,可以应用于油脂类食品中23种邻苯二甲酸酯类的同时检测.%An efficient method was established for the simultaneous determination of 23 phthalate esters residues in grease food by gas chromatography coupled with quadrupole time of flight mass spectrometry (GC-QTOF MS).The samples were extracted with Acetonitrile-methyl tertiary butyl ether (9 ∶ 1,v/v) and cleaned-up with PSA adsorbents,then determined by GC-QTOF MS and quantified by external standard method.The confirmatory analysis for target compounds was performed with the retention time and qualitative fragments obtained by data-retrieval and fragmentations.The correlation coefficients of the 23 phthalate esters were more than 0.99 in their linear ranges and the limits of quantification (LOQs) were 0.05 ～ 0.1 mg/kg.The mean recoveries for the 23 phthalate esters in grease food were between 79％ and 112％ with the relative standard deviations (RSDs,n =6) not more than 14％.The method is rapid,sensitive,and suitable for the simultaneous determination of multi-classes of phthalate esters in grease food.