高效液相色谱-串联质谱法测定焙烤食品及其塑料包装中31种邻苯二甲酸酯

建立了高效液相色谱-三重四极杆串联质谱（HPLC-MS/MS）测定焙烤食品及其塑料包装中31种邻苯二甲酸酯（PAEs）的方法。焙烤食品采用乙酸乙酯超声提取，提取液经冷冻（-18℃）、低温高速离心净化，剪碎后的塑料包装材料采用体积比为1：1：1的甲醇-丙酮-正己烷混合溶剂进行液液超声萃取后进入HPLC-MS/MS分析。采用MGⅢC₁₈色谱柱（2.0 mm×100 mm，5 μm），选择反应监测（SRM）模式测定。实验结果表明，31种邻苯二甲酸酯的特征离子质量色谱峰的峰面积与其质量浓度在各自的质量浓度范围内线性关系良好（r²≥0.9958）。样品加标回收率除邻苯二甲酸二月桂酯（DLP）为70.9%～109.7%外，其余30种化合物为80.1%～113.0%，相对标准偏差（n=6）为1.0%～13.7%。31种PAEs的检出限在0.02～8.15 μg/kg之间，定量限在0.07～27.17 μg/kg之间。应用该方法检测了面包、饼干、糕点、馅料4大类焙烤食品及其塑料包装中31种邻苯二甲酸酯的含量。该方法具有操作简单、快速、准确度和精密度高等优点，满足日常检测的要求。

Determination of 31 phthalate esters in baked foods and plastic packaging materials by high performance chromatography-tandem mass spectrometry

A high performance liquid chromatography-tandem mass spectrometric method for the analysis of 31 phthalate acid esters (PAEs) in baked foods and plastic packaging materials was developed. The food samples were extracted with ethyl acetate. Then, the extracts were frozen at -18℃, cleaned up at low temperature and high speed centrifuge before analyzed by HPLC-MS/MS. While for plastic packaging materials, after cut into small pieces, mixed solvent of methyl alcohol-acetone-n-hexane (1:1:1, v/v/v) was applied to ultra-sonic extraction of the target PAEs. The separation was performed on an MGⅢC₁₈ capillary column (2.0 mm×100 mm, 5 μm), and determined by MS/MS in selected reaction monitoring (SRM) mode. The results indicated that the method had good linear relationships with r² not less than 0.9958. The average recoveries (n=6) of the 31 PAEs were in the range of 80.1%-113.0% except for bis-dodecyl ester (DLP), whose average recoveries were 70.9%-109.7%, and the relative standard deviations were in the range of 1.0%-13.7%. The limits of detection (LODs) were 0.02-8.15 μg/kg, and the limits of quantification (LOQs) were 0.07-27.17 μg/kg. The method was successfully applied to determine the 31 PAEs in four kinds of baked foods (bread, biscuits, pastry and filling) and their plastic packaging. The method is suitable for the determination of the 31 PAEs in baked foods and packaging with easy operation, high accuracy and precision.