摘要
目的建立QuEChERS-超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)测定水产品中50种兽药残留(三苯甲烷类、酰胺醇类、硝基咪唑类、磺胺类、喹诺酮类)的方法。方法样品经过含1%甲酸的乙腈溶液提取,采用QuEChERS方法净化,通过相同C18色谱柱分离,经2个不同流动相系统(0.1%甲酸水溶液-甲醇、5mmol/L乙酸铵水溶液-甲醇)梯度洗脱后,采用UPLC-MS/MS电喷雾正离子模式、正负切换模式分别分析测定,基质添加标准曲线外标或内标法定量。结果50种药物标准曲线相关系数均>0.997,检出限为0.032~0.356μg/kg,加标回收率为60.7%~114.0%,相对标准偏差为1.06%~14.10%。结论本方法快速、高效,可应用于水产品中多种兽药残留的快速准确筛查和检测。
Objective To establish a method for the determination of 50 kinds of veterinary drugs residues(triphenylmethane,amidol,nitroimidazole,sulfonamide and quinolone)in aquatic products by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The sample were extracted with 1%formic acid in acetonitrile,purified with QuEChERS,separated by the same C18 chromatographic column,eluted by 2 different mobile phase systems(0.1%formic acid aqueous solution-methanol,5 mmol/L ammonium acetate aqueous solution-methanol),and then analyzed by UPLC-MS/MS positive ion mode and positive/negative switching mode respectively,and quantified by matrix-added calibration with external or internal standard.Results The correlation coefficients of calibration curves of 50 kinds of veterinary drugs were more than 0.997,the limits of detection were 0.032-0.356μg/kg,the average recoveries were 60.7%-114.0%,and the relative standard deviations were 1.06%-14.10%.Conclusion The method is quick and efficient,and is suitable for the determination of multi residues of veterinary drug residues in aquatic products.
作者
徐媛原
林敏霞
李凯华
钟仕花
张兵
XU Yuan-Yuan;LIN Min-Xia;LI Kai-Hua;ZHONG Shi-Hua;ZHANG Bing(Shenzhen Agricultural Product Quality and Safety Inspection and Testing Center,Shenzhen 518101,China;Key Laboratory of Edible Agricultural Product Supervision of Guangdong Market Supervision Administration,Shenzhen 518101,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2021年第16期6384-6392,共9页
Journal of Food Safety and Quality
关键词
水产品
兽药残留
QUECHERS
超高效液相色谱-串联质谱法
aquatic products
veterinary drug residues
QuEChERS
ultra performance liquid chromate graphy-tandem mass spectrometry
