TANG Xue-mei,CHEN Zhi-ting,HUANG Jian-xiang,et al.Rapid Untargeted Screening of Pesticide in Fruits and Vegetables by Ultra-performance Liquid Chromatography-High Resolution Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(12):1720-1727.
TANG Xue-mei,CHEN Zhi-ting,HUANG Jian-xiang,et al.Rapid Untargeted Screening of Pesticide in Fruits and Vegetables by Ultra-performance Liquid Chromatography-High Resolution Mass Spectrometry[J].Journal of Instrumental Analysis,2021,40(12):1720-1727. DOI: 10.19969/j.fxcsxb.21040605.
Rapid Untargeted Screening of Pesticide in Fruits and Vegetables by Ultra-performance Liquid Chromatography-High Resolution Mass Spectrometry
食品中潜在风险因子筛查对保障食品安全至关重要。该研究基于超高效液相色谱-高分辨质谱(UHPLC-HRMS)技术,提出了一种非靶向快速筛查果蔬中农药残留的策略。建立了包括样品快速前处理、UHPLC准确分离和HRMS检测在内的复杂基质中农药残留分析方法,引入保留时间校正策略,拓宽外部数据库适用度,提高定性筛查准确性。经1%乙酸乙腈提取,分散固相萃取净化后,以Accucore aQ C,18,色谱柱进行分离,通过静电场轨道阱质谱Full Scan/dd-MS,2,进行高通量定性筛查和定量检测。结果显示,不同农药在5 ~ 500 μg/L浓度范围内线性关系良好(相关系数,r,2,>, 0.99),果蔬基质添加108种代表性农药,除了矮壮素和灭蝇胺,其余农药的回收率均为61.2%~120%,相对标准偏差(RSD,,n, = 5)为0.1%~9.9%。该方法快速、准确、灵敏,适用于农产品中未知农药残留的快速筛查与定量分析。
Abstract
Screening of potential risk factors in food is very important for the ensurement of food safety.Pesticide residue is one of the important factors affecting the quality and safety of agricultural products,and the multi-residue detection of pesticides in complex matrices is still a challenging task.A rapid non-targeted screening strategy for pesticide residues in fruits and vegetables was proposed in this study,based on ultra-performance liquid chromatography-high resolution mass spectrometry(UHPLC-HRMS).Meanwhile,an analytical method for pesticide residues in complex substrates was established,including rapid sample pretreatment,accurate separation by UHPLC and detection by HRMS.Brief steps for the method construction are described as follows.Firstly,the pre-treatment method including purification agents and extraction solvents were optimized,and the acetonitrile containing 1% acetate and dispersive solid phase extraction with 20 mg PSA + 20 mg C,18, + 2.5 mg GCB + 150 mg MgSO,4, were selected for sample preparation,owing to its relatively high recoveries for most of pesticides.Secondly,the instrument conditions were optimized,the separation was performed on an Accucore aQ C,18, column,and the high-throughput qualitative screening and quantitative detection were performed by Full Scan/ dd-MS,2,.More importantly,the retention time correction strategy was introduced to calibrate the retention time generated under different LC-MS conditions.Finally,a high-resolution database containing 651 pesticides was established based on the original commercial database and the actual situation of the limits of different pesticides on agricultural products in various countries.Under the optimized conditions,108 kind of pesticides in fruit and vegetable matrix were analyzed.Results showed that there were good linear relationships for all the pesticides in the concentration range of 5-500 μg/L,with their correlation coefficients(,r,2,) larger than 0.99.The limits of detection(LODs,,S,/,N, ≥ 3) for all the pesticides were in the range of 0.002-1.5 μg/kg,while the limits of quantitation(LOQs) were 5 μg/kg.At three spiked levels of 5,25,100 μg/kg,the recoveries for 106 pesticides except cyromazine and chlormequat chloride ranged from 61.2% to 120%,with relative standard deviations(RSD) of 0.1%-9.9%.The established method was successfully applied to the analysis of fifty-eight cowpea and twelve citrus samples for pesticides screening.Results showed that this method was rapid,accurate and sensitive,and was suitable for the rapid screening and quantitative analysis of unknown pesticide residues in agricultural products.
关键词
超高效液相色谱-高分辨质谱(UHPLC-HRMS)农药残留非靶向果蔬
Keywords
ultra-performance liquid chromatography-high resolution mass spectrometry (UHPLC-HRMS)pesticide residueuntargetedfruits and vegetables
references
Wang L,Dong Y J,Fan L X,Liang J Y,Yuan X X,Zhao S C.J. Shangdong Agric. Sci. (王磊,董燕婕,范丽霞,梁京芸,苑学霞,赵善仓.山东农业科学),2019,338(10):173-178.
Liu X M,Xu X L,Nie X M,Guo W,Zhang F.Chin. J. Chromatogr. (刘晓敏,许秀丽,聂雪梅,国伟,张峰.色谱),2020,38(7):750-758.
Narenderan S T,Meyyanathan S N,Babu B.Food Res. Int.,2020,133:109141.
Screening of 166 Pesticide Residues in Tea Based on Ultra High Performance Liquid Chromatography-Quadrupole/Electrostatic Field Orbitrap High Resolution Mass Spectrometry
Determination of 35 Pesticide Residues in Green Tea by Gas Chromatography-Triple Quadrupole Mass Spectrometry
Research Progress on Rapid Detection of Pesticide Residues Based on Molecular Recognition
Related Author
No data
Related Institution
College of Chemical Engineering,Zhejiang University of Technology
Tea Research Institute,Chinese Academy of Agriculture Sciences