[关键词]
[摘要]
建立了分子印迹固相萃取(MISPE)气相色谱串联质谱法(GC-MS/MS)检测食用植物油中苯并[a]蒽(BAA)、屈(CHR)、苯并[b]荧蒽(BBF)和苯并[a]芘(BAP)等4种欧盟限量多环芳烃(PAH4)的新方法。以CHR-d12和BAP-d12为内标,样品用正己烷溶解,流过硅胶-分子印迹串联固相萃取小柱,弃去硅胶柱;分子印迹小柱再经正己烷淋洗,二氯甲烷洗脱;洗脱液经氮吹浓缩,GC-MS/MS多反应监测模式进行检测。结果表明,在1~50 μg/L浓度范围内4种PAH均有良好的线性(R2>0.999),方法检出限为0.21~0.49 μg/kg,定量限为0.70~1.63 μg/kg;5、10和20 μg/kg加标水平的回收率为81.06~111.30%,相对标准偏差为0.86~5.65%。利用本方法对市售26个食用植物油样品进行检测,结果显示,BAA、CHR、BBF和BAP的检出率均为100%;BAP含量为2.04~6.16 μg/kg;PAH4含量为9.36~31.38 μg/kg。依我国相关限量标准,BAP含量处于较安全水平,但PAH4总量较欧盟限量要求还存在较大差距。
[Key word]
[Abstract]
A new method was established based on molecular imprinting solid phase extraction and gas chromatography tandem mass spectrometry (GC-MS/MS) to determine 4 polycyclic aromatic hydrocarbons (PAH4) in edible oil limited by EU, including benz (a) anthrancene (BAA), chrysene (CHR), benzo (b) fluoranthene (BBF) and benzo (a) pyrene (BAP). . The edible vegetable oil sample was dissolved by n-hexane with CHR-d12 and BAP-d12 as internal standards, and then the sample solution was passed through a BAP molecularly imprinted cartridge connected a silica gel cartridge above. After discarding the silica gel cartridge, the molecularly imprinted cartridge was rinsed with n-hexane and eluted with dichloromethane. The eluent solution was concentrated with nitrogen flow, and the detection was performed using GC-MS/MS MRM mode. All analysis showed that 4 PAH had good linearity (R2>0.999) in the range of 1~50 μg/L. The limits of detection and quantitation of PAH4 were 0.21-0.49 μg/kg and 0.70-1.63 μg/kg, respectively. The recovery rate of spiked levels at 5, 10 and 20 g/kg was 81.06-111.30%, and the relative standard deviation was 0.86 -5.65%. -. The results showed that BAA, CHR, BBF and BAP were detected in all the 26 commercial edible vegetable oil samples. The content of BAP was 2.04 ~ 6.16 μg/kg, and the content of PAH4 was 9.36 - 31.38 μg/kg. According to the Chinese national food safety standard, the content of BAP was in the safety level, but the total amount of PAH4 should be controlled for improving the safety quality according to the European Union limit standard.
[中图分类号]
[基金项目]
北京市教委项目(PXM2014-014207-000001);北京农学院实验技术体系基金项目(1086716287)