超高效液相色谱-高分辨质谱法测定蜂蜜中14种农药残留  

Determination of 14 pesticide residues in honey by ultra high performance liquid chromatography-high resolution mass spectrometry

作　　者：张烁[1] 陈达炜[1] 赵云峰[1] 

机构地区：[1]国家食品安全风险评估中心卫生部食品安全风险评估重点实验室,北京100021

出　　处：《卫生研究》2015年第3期422-426,430,共6页Journal of Hygiene Research

基　　金：国家国际科技合作专项(No.2011DFA31770)

摘　　要：目的建立超高效液相色谱-高分辨质谱同时快速测定蜂蜜中14种农药残留的方法。方法样品采用1%甲酸乙腈提取,以N-丙基乙二胺（PSA）和C18作为吸附剂的分散固相萃取法（d-SPE）进行净化,以Accucore aQ C18色谱柱（2.6μm,2.1 mm×150 mm）进行色谱分离,通过高分辨质谱的全扫描/实时二级质谱扫描模式进行定性筛查和定量检测。结果 14种农药残留在一定浓度范围内呈良好的线性关系,相关系数（r）均大于0.998,定量限（LOQ）为0.6-6μg/kg。空白蜂蜜样品在LOQ、15和30μg/kg三个加标水平的平均回收率为80.3%-112.7%,相对标准偏差为0.4%-7.1%。结论该方法适合蜂蜜中农药多残留的快速筛查和定量。Objective To establish a method for simultaneous determination of 14 pesticide residues in honey by ultra high performance liquid chromatography-high resolution mass spectrometry （UPLC-HRMS）. Methods Honey samples were extracted with 1% formic acid in acetonitrile, and the extracts were cleaned up with dispersive solid phase extraction （d-SPE） using the mixture of PSA and C18 powder as sorbents. The extract components were separated on an Accucore aQ C18 column（2.6μm,2.1 mm×150 mm） by gradient elution. The qualitative and quantitative analyses were operated under Full Scan/ddms2 mode by high resolution mass spectrometry. Results The response of each pesticides showed a good linearity with the correlation coefficient not less than O. 998. The limits of quantitation （LOQs, S/N≥ 10） for the 14 pesticides in honey were from 0. 6 to 6 μg/kg. The recovery results with spike blank honey samples at the levels of LOQs, 15 and 30 μg/kg were satisfied with average recovery rates of 80.3%-112.7% and the RSDs of 0.4%-7.1%. Conclusion The proposed method was suitable for the rapid screening and quantitative analysis of pesticide residues in honey.

关 键 词：分散固相萃取 高分辨质谱 蜂蜜 农药残留 

分 类 号：R155.51[医药卫生—营养与食品卫生学] TS207.53[医药卫生—公共卫生与预防医学]