改良QuEChERS-超高效液相色谱-串联质谱法测定乌鸡肉中35种兽药残留  

Determination of Thirty-five Veterinary Drug Residues in Black Chicken by Modified QuEChERS-Ultra High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：季宝成 杨澜瑞 程迎新 侯铸琛 吕佳 许旭 白艳红 JI Bao-cheng;YANG Lan-rui;CHENG Ying-xin;HOU Zhu-chen;LV Jia;XU Xu;BAI Yan-hong(College of Food and Bioengineering,Zhengzhou University of Light Industry,Zhengzhou 450001,China;Key Laboratory of Cold Chain Food Safety Quality and Safety Control in Henan Province,Zhengzhou 450001,China;Key Laboratory of Cold Chain Food Processing and Safety Control(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,河南郑州450001 [2]河南省冷链食品安全质量安全控制重点实验室,河南郑州450001 [3]冷链食品加工与安全控制教育部重点实验室(郑州轻工业大学),河南郑州450001

出　　处：《质谱学报》2023年第6期807-819,I0004,共14页Journal of Chinese Mass Spectrometry Society

基　　金：国家自然科学基金青年科学基金项目(32202174,31901767);河南省重大公益专项(201300110100);2022年河南省重点研发与推广专项科技攻关项目(232102321118);郑州轻工业大学博士科研基金资助项目(13501050079);郑州轻工业大学星空众创空间创新培育项目(2023ZCKJ205)。

摘　　要：本研究建立了以还原氧化石墨烯改性三聚氰胺海绵(r-GO@MeS)作为基质净化材料的改良QuEChERS法,结合高效液相色谱-串联质谱(UPLC-MS/MS)法快速测定乌鸡肉中35种兽药残留。考察了金属螯合剂(Na2EDTA)、脱水剂种类(MgSO_(4)、Na_(2)SO_(4))与乙酸添加量(0%、0.5%、1%、3%、5%)对待测兽药提取效果的影响,探究了海绵用量与净化模式(动态与静态)对待测兽药净化效果的影响。与常用的基质净化材料(C18、PSA、GBC)对比发现,r-GO@MeS具有同等甚至更优的净化效果和便捷度。方法学考察结果表明,在50、100、150μg/kg 3个加标水平下,监测药物回收率为66.6%~118.8%;日内、日间精密度分别小于13.8%和14.6%;在5~200μg/kg浓度范围内,线性关系良好(R^(2)≥0.998)、基质效应低(-19.4%~19.8%)、检出限(LOD)和定量限(LOQ)分别为0.1~6μg/kg和0.3~15μg/kg。该方法操作简便、成本较低,在兽药多残留检测领域具有较好的应用价值。In this study,a modified QuEChERS(Quick,Easy,Cheap,Effective,Rugged,and Safe)method with using a reduced graphene oxide-modified melamine sponge(r-GO@MeS)as matrix purification material was developed for the determination of 35 veterinary drug residues in black chicken meat by ultra-high-performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).First of all,the effects of metal chelating agents(Na 2EDTA),dehydrating agents(MgSO_(4),Na_(2)SO_(4))and acetic acid(HAc)addition(0%,0.5%,1%,3%,5%)on the extraction efficiency of veterinary drugs were thoroughly studied.According to the results,most of quinolones tended to chelate with magnesium ions,resulting in low recoveries of veterinary drugs in the extraction solution,while the appropriate addition of Na 2EDTA and HAc could improve the overall drug recoveries.Therefore,2.5 mL of 0.1 mmol/L Na 2EDTA aqueous solution and 10 mL of 0.5%HAc-ACN were used as extraction solvents,with 2.0 g of anhydrous Na_(2)SO_(4)and 0.5 g of NaCl as dehydrating agents.Then the effects of sponge dosages(sponge volume/extract volume of 0.45,0.60,0.75,0.90,1.05 cm^(3)/mL)and different purification modes(dynamic cycles of 1,5,10,static time of 1,5,10 min)on the purification efficiency were investigated in terms of veterinary drug recoveries.The results showed that a moderate dosage of 0.75 cm^(3)/mL and fast ten dynamic purification cycles tended to give out more acceptable recoveries for all drugs.The method validation results showed that the recoveries of all monitored drug were obtained in the range of 66.6%-118.8%with three different spiked levels of 50,100,150μg/kg.The intra-and inter-day precisions were evaluated in terms of relative standard deviations(RSDs)by repeatability tests conducted on the same day or three consecutive days,which were acquired less than 13.8%and 14.6%,respectively.In the range of 5-200μg/kg,good linearities were acquired with the correlation coefficients(R^(2))no less than 0.998.Additionally,the limits of detection(LODs)and quantitation(LOQs)were

关 键 词：QUECHERS 氧化石墨烯 三聚氰胺海绵 兽药 乌鸡肉 液相色谱-串联质谱(LC-MS/MS) 

分 类 号：O657.63[理学—分析化学]