基于还原氧化石墨烯改性三聚氰胺海绵的改良QuEChERS-超高效液相色谱-串联质谱法快速测定鸡蛋中32种兽药残留  

Rapid Determination of 32 Kinds of Veterinary Drug Residues in Eggs Using Modified QuEChERS Based on Reduced Graphene Oxide-coated Melamine Sponge by Ultra-High Liquid Chromatography-Tandem Mass Spectrometry

作　　者：许旭 吕佳 杨澜瑞 侯铸琛 季宝成 白艳红 XU Xu;LYU Jia;YANG Lan-Rui;HOU Zhu-Chen;JI Bao-Cheng;BAI Yan-Hong(College of Food and Bioengineering,2 Key Laboratory of Cold Chain Food Safety Quality and Safety Control in Henan Province,3 Key Laboratory of Cold Chain Food Processing and Safety Control,Ministry of Education,Zhengzhou University of Light Industry,Zhengzhou 450001,China)

机构地区：[1]郑州轻工业大学食品与生物工程学院,郑州450001 [2]郑州轻工业大学河南省冷链食品安全质量安全控制重点实验室,郑州450001 [3]郑州轻工业大学冷链食品加工与安全控制教育部重点实验室,郑州450001

出　　处：《分析化学》2024年第1期121-129,共9页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金项目(Nos.32202174,31901767);河南省高等学校重点科研项目(No.24A550021);河南省重点研发与推广专项项目(No.232102321118)资助。

摘　　要：基于还原氧化石墨烯改性三聚氰胺海绵(r-GO@MeS)的改良QuEChERS技术,建立了一种超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定鸡蛋中32种兽药多残留的快速分析方法。考察了石墨烯改性浓度、海绵用量及净化模式对净化过程兽药回收率的影响,筛选出最佳净化条件为:采用改性浓度为0.5 mg/mL的r-GO@MeS,海绵用量为6.0 cm^(3)/mL,动态挤压5次。以RRHD C18色谱柱分离,采用电喷雾离子源(ESI),在多反应监测模式(MRM)下,用外标法进行定量分析。32种兽药的线性相关系数(R^(2))均大于0.999,基质效应(ME)为–7.8%~18.9%,检出限(LODs,S/N≥3)为0.2~10.2μg/kg,定量限(LOQs,S/N≥10)为0.6~28.0μg/kg,低、中、高3个加标水平下的回收率在66.5%~117.5%范围内,日内和日间精密度(RSD)分别为13.3%和16.3%。本研究所开发的r-GO@MeS制备过程简单,基质净化过程便捷、高效,无需高速离心以及强磁场辅助等步骤,显著缩短了样品前处理时间。建立的改良QuEChERS技术结合UPLC-MS/MS的方法适用于鸡蛋中兽药多残留的同时快速检测。A rapid analytical method for simultaneous determination of 32 kinds of multi-residue veterinary drugs in eggs was developed using a modified QuEChERS technique based on a reduced graphene oxide-coated melamine sponge(r-GO@MeS)by ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The influences of graphene oxide(GO)concentrations,sponge dosages,and purification modes on drug recoveries were investigated during the purification process.The optimal purification conditions involved using a GO concentration of 0.5 mg/mL,a sponge dosage of 6.0 cm^(3)/mL,and a dynamic purification mode of 5 extrusion cycles.Separation was achieved using an Agilent Eclipse Plus C18 RRHD column(100 mm×2.1 mm,1.8μm),and quantitative analysis was performed by the external standard method using an electrospray ionization source(ESI)in multiple reaction monitoring(MRM)mode.The results showed that all 32 kinds of veterinary drugs exhibited good linear correlation with coefficients greater than 0.999,and matrix effects(MEs)ranging from‒7.8%to 18.9%.The limits of detection(LODs)and quantification(LOQs)ranged from 0.2 to 10.2μg/kg and from 0.6 to 28.0μg/kg,respectively.The recoveries for the three spiked levels were in the range of 66.5%‒117.5%,with intraday and inter-day precision(Relative standard deviation)below 13.3%and 16.3%,respectively.The synthetic r-GO@MeS exhibited efficient matrix purification without the need of high-speed centrifugation or strong magnetic field assistance.This significantly shorted the sample pretreatment time and improved the convenience of the matrix purification process.Combined with UPLC-MS/MS,the method was suitable for the rapid determination of multi-residue veterinary drugs in eggs.

关 键 词：兽药 鸡蛋 氧化石墨烯 三聚氰胺海绵 液相色谱-串联质谱 

分 类 号：O657.63[理学—分析化学] TS253.7[理学—化学]