QuEChERS法净化联用UPLC-MS/MS分析鸡肉、蛋中22种药物的残留  

Simultaneous determination of residues of 22 kinds of veterinary drugs in chicken and egg by QuEChERS combined with UPLC-MS/MS

作　　者：于霞 马凯 简银池 吴新文 黄永桥 王乾丽 王莉娜 曹俊杰 YU Xia;MA Kai;JIAN Yinchi;WU Xinwen;HUANG Yongqiao;WANG Qianli;WANG Lina;CAO Junjie(Guizhou Testing Technology Research and Application Center,Guiyang 550014,China;Guizhou Academy of Testing and Analysis,Guiyang 550014,China)

机构地区：[1]贵州省检测技术研究应用中心,贵州贵阳550014 [2]贵州省分析测试研究院,贵州贵阳550014

出　　处：《贵州科学》2025年第1期78-85,共8页Guizhou Science

摘　　要：创建了QuEChERS法净化联用UPLC-MS/MS分析鸡肉、蛋中磺胺类、喹诺酮类和四环素类22种药物残留量的方法。样品经Na2EDTA-Mcllvaine缓冲溶液和6%甲酸乙腈提取、盐析和净化后上机分析。以C18色谱柱分离,以0.1%甲酸乙腈和0.1%甲酸水含2 mmol·L^(-1)乙酸铵溶液为流动相,梯度洗脱,电喷雾离子源(ESI^(+))扫描,结合动态多重反应监测(MRM)模式,用外标法定量。22种兽药的线性范围好,相关系数(r)全都大于0.995,检出限(LOD)在0.5~1.0μg·kg^(-1)范围,定量限(LOQ)在1.5~3.0μg·kg^(-1)范围;高、中、低3个浓度水平下开展加标回收试验,其中回收率在76.6%~107.2%范围,相对标准偏差(RSD)在1.8%~11.6%范围。通过对实际样品的检测,本方法高效、快捷、灵敏、可靠、经济和通量高,适合对鸡肉和鸡蛋中的磺胺类(Sulfonamides)、喹诺酮类(Quinolones)及四环素类(Tetracyclines)兽药残留进行分析检测。A method for simultaneous determination of the residues of 22 kinds of veterinary drugs in chicken and eggs was established by QuEChERS combined with UPLC-MS/MS.The samples were dissolved in Na 2EDTA-Mcllvaine buffer and extracted by 6%formate acetonitrile,and salination and purification were performed before analysis.C 18 column was used for separation,with 0.1%formic acid acetonitrile and 0.1%formic acid 2 mmol/L ammonium acetate water solution as the mobile phase for gradient elution.The samples were scanned by high voltage electrospray ionization mass spectrometry(ESI^(+))under dynamic multiple response detection(MRM)mode,and quantified by external standard method.The 22 kinds of veterinary drugs had good linear relationship,with correlation coefficients greater than 0.995.The detection limits were between 0.5μg/kg and 1.0μg/kg,and the quantitative limits were between 1.5μg/kg and 3.0μg/kg.The spiked recovery rates were between 76.6%and 107.2%,and the relative standard deviation(RSD)was between 1.8%and 11.6%.Through the detection of actual samples,the method was proved to be efficient,fast,sensitive,reliable,and economical,suitable for the determination of veterinary drugs in chicken and eggs such as sulfonamides,quinolones,and tetracyclines.

关 键 词：QuEChERS法 UPLC-MS/MS 鸡肉 鸡蛋 22种兽药Quinolones 

分 类 号：O657[理学—分析化学]