比较3种不同前处理方法结合高分辨质谱测定姜中农药残留的效果  

Comparison of the effects of 3 kinds of different pretreatment methods combined with high-resolution mass spectrometryapplied to the determination of pesticide residues in ginger

作　　者：韩梅[1] 郭灵安[1] 焦颖 邱世婷[1] 贺光云 李莹 覃蜀迪 HAN Mei;GUO Ling-An;JIAO Ying;QIU Shi-Ting;HE Guang-Yun;LI Ying;QING Shu-Di(Institute of Quality Standard and Testing Technology for Agro-products,Sichuan Academy of Agricultural Sciences/Laboratory of Risk Assessment for Agricultural Product(Chengdu),Ministry of Agriculture and Rural Affairs,Chengdu 610066,China)

机构地区：[1]四川省农业科学院农业质量标准与检测技术研究所,农业农村部农产品质量安全风险评估实验室(成都),成都610066

出　　处：《食品安全质量检测学报》2021年第9期3674-3683,共10页Journal of Food Safety and Quality

基　　金：国家蔬菜产品质量安全风险评估项目(GJFP2019009)。

摘　　要：目的采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法测定姜中农药残留,对比3种不同前处理方法对测定结果的影响。方法分别从基质效应、净化效果、回收率和定量限等方面考察未净化法、QuEChERS前处理法、氨基柱固相萃取法(solid-phase extraction,SPE)3种不同前处理方法的提取效果。结果经未净化法、QuEChERS法和SPE法处理后,在姜中表现为无基质效应的农药占比分别为0%、4%、21.6%。SPE法具有较好的净化效果,基质效应小,但操作较繁琐费,且一部分农药回收率低于70%。未净化法和QuEChERS方法简单高效,适用于大批量样品进行检测,同时能保证大多数农药回收率在70%~120%之间。结论3种前处理方法各有优势,在检测分析中,可根据不同需要选择前处理方法。Objective To determine the pesticide residues in ginger by ultra performance liquid chromatography-quadrupole/orbitrap high-resolution mass spectrometry,and compare the effects of 3 kinds of different pretreatment methods on the determination results.Methods The extraction effects of 3 kinds of different pretreatment methods,namely the unpurification method,QuEChERS pretreatment method,and solid-phase extraction(SPE),were investigated from the aspects of matrix effect,purification effect,recovery rate and quantification limit.Results The proportions of pesticides which showed no matrix effect in ginger by the method of unpurification,QuEChERS and SPE were 0%,4%and 21.6%respectively.SPE method had good purification effect,and the matrix effect was small,but the operation was more complicated,and the recovery rate of some pesticides was less than 70%.The methods of unpurification and QuEChERS were simple and efficient,and they were suitable for large-scale samples detection,and could ensure that the recoveries of most pesticide were between 70%and 120%.Conclusion The 3 kinds of pre-treatment methods have their own advantages.In the detection and analysis,the pretreatment methods can be selected according to different needs.

关 键 词：农药残留 姜 未净化法 Qu ECh ERS 固相萃取法 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法 

分 类 号：O657.63[理学—分析化学] TS207.53[理学—化学]