油料作物由于含油量高、基质复杂,导致其弱极性多环芳烃类化合物提取率低,成为准确检测高油样品中多环芳烃的瓶颈.本文对比了16种多环芳烃的GC-MS/MS检测条件SIM(Single Ion Monitoring)模式和SRM(Se-lective Reaction Monitoring)模式质谱信号响应,SRM模式干扰峰更少,检出限更低;对比了QuEChERS和超声辅助提取方法对大豆、油菜籽、花生三种油料中16种多环芳烃的提取效果,超声辅助提取的基质效应很高,部分多环芳烃基质减弱80%以上,且油菜籽的提取稳定性差,部分相对标准偏差达到32%～45%.并比较了乙腈和丙酮作为QuCEhERS方法提取溶剂的提取效果.结果表明,QuCEhERS方法中乙腈作为提取溶剂,在极性最弱的多环芳烃回收率低,如苯并[b]荧蒽、苯并[k]荧蒽等,回收率甚至小于10%.而丙酮作为QuCEhERS方法提取溶剂,而在极性弱的多环芳烃中,回收率提高了3～5倍,适合提取高油样品中多环芳烃.三种油料基质匹配标准曲线的相关系数均在0.99以上.16种多环芳烃均能获得较好的回收率(58%～100%),相对标准偏差为0.4%～10.6%,方法稳定性好.
Optimization of dispersive solid-phase extraction method of polycyclic aromatic hydrocarbons in oil crops detected by GC-MS
Due to the high oil content and complex matrix,the extraction rate of weak polar polycyclic aromatic hydrocarbons(PAHs)from oil crops is low,which becomes the bottleneck of accurate detection of PAHs in high oil samples.In this paper,the mass spectrum signal responses of 16 PAHs were compared between GC-MS/MS detec-tion condition--SIM(Single Ion Monitoring)mode and Selective Reaction Monitoring(SRM)mode.The SRM mode has less interference peak and lower detection limit.The extraction effects of QuEChERS and ultrasound-as-sisted extraction methods on 16 PAHs from soybean,rapeseed and peanut were compared.The matrix effect of ultra-sound-assisted extraction was high,some PAHs matrix was reduced by more than 80%,and the extraction stability of rapeseed was poor,and some relative standard deviations reached 32%-45%.The extraction effects of acetoni-trile and acetone as QuCEhERS were compared.The results showed that acetonitrile was used as extraction solvent in QuCEhERS method,and the recovery of polycyclic aromatic hydrocarbons with the weakest polarity was low,such as benzo-fluoranthrene and benzo-fluoranthrene,and the recovery was even less than 10%.Acetone was used as the solvent to extract PAHs,and the recovery rate of PAHs with weak polarity was improved by 3-5 times,which was suitable for extracting PAHs from high oil samples.The correlation coefficients of three oil matrix matching standard curves are all above 0.99.The recoveries of 16 PAHs were 58%～100%,and the relative standard devia-tions were 0.4%～10.6%.The method had good stability.
万方数据
维普
