食品接触材料中邻苯二甲酸酯的LTQ-Orbitrap组合式高分辨质谱快速筛查和确证

建立了食品接触材料中邻苯二甲酸酯快速筛查确证的高效液相色谱-高分辨质谱法(HPLC-LTQ-Orbi-trap/MS)。实验中采用加速溶剂萃取(ASE)法为样品前处理手段,优化了萃取溶剂、萃取温度、静态萃取时间等实验参数,提高了食品接触材料中邻苯二甲酸酯的提取效率。采用高分辨质谱有效地去除了基体干扰,通过静电场轨道阱全扫描得到的精确相对分子质量进行了化合物的定量,用离子阱的二级质谱图对未知化合物进行了进一步确证。结果表明:邻苯二甲酸酯的检测限为1 ng/mL;该方法的加标回收率为89.8%～101.3%,相对标准偏差均小于8.0%;所建立的方法简单,灵敏度高,适用于食品接触材料中邻苯二甲酸酯类增塑剂的筛查和检测。

Screening and Confirmation of Phthalates in Food Contact Materials by Hybrid Linear Ion Trap/Orbitrap Mass Spectrometry

A fast screening and conformation method of phthalates in food contact materials based on liquid chromatography mass spectrometry using a linear ion trap-orbitrap hybrid instrument at high mass resolution(HPLC-LTQ-Oribitrap/MS) was developed.Accelerated solvent extraction method was applied for pretreatment of specimen.The operational parameters of ASE were optimized,such as extraction solvent,extraction temperature,static extraction time,flush volume and extraction cycles,to improve extraction efficiency of phthalates from food contact materials.High resolution mass spectrometry was applied to remove matrix interference.Full scanning of electrostatic field orbitrap was applied for quantification of compounds.Secondary mass spectrometric image of ion trap was applied to verify the unknown compounds.The results showed that the detection limit of phthalates were 1 ng/mL;the average recoveries is from 89.8% to 101.1%,with RSDs less than 8.0%.It was concluded that the method is simple,sensitive,and suitable for screening and confirmation of PAEs in food contact materials.