联合净化法结合高效液相色谱-串联质谱同时测定鸽蛋中5类24种兽药残留  

Simultaneous Determination of 5 Kinds of 24 Veterinary Drug Residues in Pigeon Eggs by Combined Purification Method Coupled with High Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：张静[1] 马丽娜[1] 刘茵茵[1] 周倩[1] 唐修君[1] 陆俊贤[1] 樊艳凤[1] 赵敏 高玉时[1] ZHANG Jing;MA Li'na;LIU Yinyin;ZHOU Qian;TANG Xiujun;LU Junxian;FAN Yanfeng;ZHAO Min;GAO Yushi(Jiangsu Institute of Poultry Science,Yangzhou,Jiangsu 225125)

机构地区：[1]江苏省家禽科学研究所,江苏扬州225125

出　　处：《中国家禽》2025年第2期105-112,共8页China Poultry

基　　金：扬州市社会发展项目(YZ2022066);江苏省种业振兴揭榜挂帅项目(JBGS[2021]107);江苏省农业科技自主创新资金(CX(21)2011)。

摘　　要：为建立一种可同时检测鸽蛋中多类兽药残留的高通量液相色谱-串联质谱法,试验采用正己烷去脂,联合QuEChERS净化结合冷冻脂质过滤法,建立检测鸽蛋中5类24种兽药残留的高效液相色谱-串联质谱法。样品中的5类兽药(氯霉素类、磺胺类、硝基咪唑类、喹诺酮类和抗病毒类)经1.0%乙酸乙腈溶液提取,氮气吹干,冷冻过夜后,结合QuEChERS净化和正己烷去脂,采用1 mL 0.1%甲酸水-乙腈溶液(v/v,90∶10)复溶;高效液相色谱-串联质谱测定,内标法定量,采用实际样品建立方法的初步应用。结果显示:24种兽药在2.0~200 ng/mL线性关系良好(R2>0.99),该方法的定量限为2μg/kg,平均回收率为62.2%~117.1%,相对标准偏差4.3%~18.9%;实际样品检出的7种目标化合物与标准方法相比的相对标准偏差为1.34%~5.20%。研究表明,建立的检测鸽蛋中多类兽药残留的高通量液相色谱-串联质谱法省去固相萃取步骤,成本较低,灵敏高效,回收率优良、重复性稳定,适用于鸽蛋中多类兽药的快速监测分析。To establish a method for the determination of veterinary drug residues in pigeon eggs by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS),samples were extracted and purified using frozen lipid filtration combined with the QuEChERS method taking advantage of n-hexane liquid purification.A total of 24 veterinary drugs encompassing 5 classes of drug(chloramphenicols,sulfonamides,nitroimidazoles,quinolones and antiviral)in pigeon eggs were analyzed.The drugs were extracted in 1.0%acetic acid acetonitrile(v/v),dried with nitrogen and frozen at very low temperature.The drugs were diluted by mobile phases,and cleaned using frozen lipid filtration and n-hexane liquid purification.The separation of residue targets was performed with a gradient elution of 0.1%(v/v)formic acid aqueous solution and acetonitrile(v/v,90/10)as mobile phases and detected by HPLC-MS/MS by the internal standard method.The method was preliminarily applied with actual samples.The results showed that this method gave good linearity within a certain concentration range(R2>0.99),and the acceptable limit of quantification was 2.0μg/kg,and the average recovery rate was from 62.2%to 117.1%,relative standard deviation was ranged from 4.3%to 18.9%for the 24 veterinary drugs.The relative standard deviations of 7 target compounds were from 1.34%to 5.20%compared with the standard method.The results indicated that the established HPLC-MS/MS proved suitable for the rapid determination of veterinary drugs residues in eggs with a simple,accurate,and low-cost procedure,and omitted the solid phase extraction.

关 键 词：联合净化法 高效液相色谱-串联质谱 QUECHERS 兽药残留 鸽蛋 

分 类 号：S859.84[农业科学—临床兽医学]