大气压化学电离-液相色谱串联质谱法测定油基食品中的18种邻苯二甲酸酯类化合物

Determination of 18 Phthalic Acid Esters Compounds in Oily Foodstuffs by Atmospheric Pressure Chemical Ionization (APCI) Liquid Chromatography Tandem Mass Spectrometry

摘要:

根据2011年6月卫生部公示的食品中17种禁用邻苯二甲酸酯的名单，本方法采用相色谱-串联四极杆质谱建立了快速测定含油食品中18种邻苯二甲酸酯( PAEs)含量的分析方法。食品采用乙腈提取，加入水稀释后，正己烷液液萃取，样液浓缩至干后，甲醇定容。采用C18液相色谱柱分别在等度与梯度两种洗脱程序下分离，大气压化学正离子电离，多反应监测模式测定。在该优化方法条件下，18种邻苯二甲酸酯检测限（LOQ）在0.05~0.5 mg/kg之间，方法回收率为53.4%~107.9%，相对标准偏差（RSD）为7.2%~24.6%。应用本方法分析了植物油、起酥油、辣椒酱、豆辨酱、饼干等多种食品中18种邻苯二甲酯类物质含量，经与标准方法相比，表明本方法操作简单、测定结果准确，可以作为食品中18种邻苯二甲酸酯类化合物的确证方法。

Abstract:

A quick confirmative method was developed for determining 18 phthalic acid esters (PAEs) in oily foodstuffs by liquid chromatography tandem quadrupole mass spectrometry (LC-MS/MS), basing on the ministry of health announcement about 17 illegal PAEs in foodstuffs. The oil sample was extracted with acetonitrile. After mixed with water, n-hexane was selected as the solvent of liquid-liquid extraction. The extracts were concentrated to dry and methanol was used to dissolve residues. The separation was carried out on C18 column with the isocratic and gradient elution. The detection of 18 analytes was achieved in the positive atmosphere pressure chemical ionization (APCI) and multi-reaction monitoring (MRM) mode. With the optimized condition, the limits of quantification (LOQ) of the 18 PEAs analytes were 0.05-0.5 mg/kg. The overall recovery varies from 53.4% to 107.9%, and the relative standard deviations (RSD) were between 7.2% and 24.6%. Real sample including vegetable oil, shortening oil, chili sauce, bean sauce, and biscuit were determined 18 PAEs residues with this method and compared with the standard method. The results showed that the method was simple, accurate and suitable for the determination of 18 PAEs in oily foodstuffs.