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

中文关键词:  气相色谱-串联质谱法  多环芳烃  固相萃取  蔬菜

英文关键词:gas chromatography-tandem mass spectrometry  polycyclic aromatic hydrocarbons  solid-phase extraction  vegetables

中文摘要:

      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/mL范围内呈线性关系良好, 方法的检出限(S/N=3)为0.09~0.51 μg/kg, 定量限(S/N=10)为0.31~1.68 μg/kg。在2、5、20 μg/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。

英文摘要:

      Objective To establish a 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 0.51 μg/kg, and limits of quantification (LOQs, S/N=10) ranged from 0.31 to 1.68 μg/kg. The average recoveries at 3 spiked levels of 2, 5, 20 μg/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.