固相萃取-气相色谱-串联质谱法测定蔬菜中的16种多环芳烃  

Determination of 16 kinds of polycyclic aromatic hydrocarbons in vegetables by solid phase extraction-gas chromatography-tandem mass spectrometry

作　　者：王敬[1] 项佳林[1] 韩林[1] 赵赴[1] 艾连峰[1] 

机构地区：[1]河北出入境检验检疫局,石家庄050051

出　　处：《食品安全质量检测学报》2016年第12期4878-4885,共8页Journal of Food Safety and Quality

基　　金：河北出入境检验检疫局科技项目(HE2014K053)~~

摘　　要：目的建立固相萃取-气相色谱-串联质谱法测定蔬菜中16种多环芳烃（polycyclic aromatic hydrocarbons,PAHs）的分析方法。方法样品经正己烷-二氯甲烷匀浆提取,经中性硅胶-中性氧化铝复合固相萃取柱净化后,用多反应监测（multiple-reaction monitoring,MRM）正离子扫描方式进行检测,气相色谱-串联质谱法测定,内标法定量。结果 16种目标物在2~250 ng/m L范围内呈线性关系良好,方法的检出限（S/N=3）为0.09~0.51μg/kg,定量限（S/N=10）为0.31~1.68μg/kg。在2、5、20μg/kg 3个加标水平下的平均回收率为添加平均回收率范围为70.6%~109.2%,相对标准偏差（RSD）为1.95%~10.4%。结论该方法选择性好、抗干扰能力强,能满足国内外法规的要求,可用于蔬菜中多环芳烃残留的日常检测。Objective To establisha method for the simultaneous determination of 16 kinds of polycyclic aromatic hydrocarbons （PAHs） in vegetables by solid phase extraction-gas chromatography-tandem mass spectrometry.Methods Samples were dissolved in n-hexane and dichloromethane, cleaned-up by silica-alumina composite solid-phase extractor, and determined by gas chromatography-tandem mass spectrometry （GC-MS/MS） using internal standard method with positive polarity mode under multiple-reaction monitoring （MRM） scan type. Results The method showed good linearity in the range of 2~250 ng/mL. The limits of detection （LODs,S/N=3） were in the range of 0.09 to 0.51μg/kg, and limits of quantification （LOQs,S/N=10） ranged from 0.31 to 1.68μg/kg. The average recoveries at 3 spiked levels of 2, 5, 20μg/kg were in the range of 70.6%~109.2%, with relative standard deviations （RSDs） of 1.95%~10.4%.Conclusion This method is selective without interference and reliable for meeting the requirements of the domestic and international legislation, and can be used for the routine analysis of PAHs in vegetables.

关 键 词：气相色谱-串联质谱法 多环芳烃 固相萃取 蔬菜 

分 类 号：TS255.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]