超高效液相色谱-串联质谱法测定鸡肉中头孢拉定残留  

Determination of Cephradine Residues in Chicken by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

作　　者：金晓峰[1] 焦仁刚[1] 赵贵[1] 栾庆祥[1] 黄鑫[1] 章厉劼[1] 王庆红[1] 孙真峥 黄瑾[1] 周光华 雷学昌 JIN Xiaofeng;JIAO Rengang;ZHAO Gui;LUAN Qingxiang;HUANG Xin;ZHANG Lijie;WANG Qinghong;SUN Zhenzheng;HUANG Jin;ZHOU Guanghua;LEI Xuechang(Guizhou Provincial Veterinary Drug and Feed Supervision Institute,Guiyang 550003;Qianxinan State Animal Products Quality and Safety Inspection Station,Xingyi 562400;Qiannan State Agri-Products Quality and Safety Supervision Inspection Center,Duyun 558013)

机构地区：[1]贵州省兽药饲料监察所,贵州贵阳550003 [2]黔西南州畜牧水产品质量安全检测站,贵州兴义562400 [3]黔南州农产品质量安全监督综合检测中心,贵州都匀558013

出　　处：《分析科学学报》2020年第3期410-414,共5页Journal of Analytical Science

基　　金：贵州省科技计划(黔科合支撑[2019]2318号);贵州省农业农村厅科技项目(No.GZ2020JQFX0101)。

摘　　要：建立测定鸡肉中头孢拉定残留的超高效液相色谱-串联质谱分析方法。鸡肉样品经80%乙腈水溶液提取,PRiME HLB柱固相萃取净化,0.2%甲酸水溶液稀释,采用Waters ACQUITY UPLC HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离,以0.1%甲酸-0.1%甲酸乙腈为流动相,梯度洗脱,基质加标外标法定量。实验结果表明,头孢拉定在0.5~50.0 ng/mL浓度范围内呈良好的线性关系(R2=0.9998),定量限为1μg/kg。向空白鸡肉中添加头孢拉定含量为1.00μg/kg、2.00μg/kg、10.0μg/kg时,回收率在77.3%~106.8%之间,相对标准偏差在3.2%~10.5%之间。本方法操作简便、快捷,实验结果准确、稳定,可满足鸡肉中头孢拉定残留量的检测。A method for the determination of cephradine residues in chicken by ultra-high performance liquid chromatography-mass spectrometry/mass spectrometry has been developed.Chicken was extracted by 80% acetonitrile,purified by PRiME HLB solid phase extraction,diluted by 0.2% formic acid,quantified by matrix external standard method,and determined by UPLC-MS/MS.The results showed that there was a good linear relationship in the range of 0.5-50.0 ng/mL(R^2=0.9998).Meanwhile,the recoveries of cephradine ranged from 77.3% to 106.8% at three concentration levels(1.00,2.00,10.0 μg/kg),the relative standard deviations were 3.2%-10.5%,and the quantitative limit was 1 μg/kg.This method is simple,rapid,accurate and stable,and meets the requirement for the determination of cephradine residues in chicken.

关 键 词：鸡肉 头孢拉定 超高效液相色谱-串联质谱 兽药残留 

分 类 号：O657.63[理学—分析化学]