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.
作者
金晓峰
焦仁刚
赵贵
栾庆祥
黄鑫
章厉劼
王庆红
孙真峥
黄瑾
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)
出处
《分析科学学报》
CAS
CSCD
北大核心
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)。
关键词
鸡肉
头孢拉定
超高效液相色谱-串联质谱
兽药残留
Chicken
Cephradine
Ultra-high performance liquid chromatography-mass spectrometry/mass spectrometry
Veterinary drug residues
