摘要
为了检测水产品中硝基咪唑类药物及其代谢物,建立了甲硝唑、地美硝唑、洛硝达唑、羟基甲硝唑、羟甲基甲硝咪唑残留量的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法,样品经过含0.2%甲酸的乙腈水溶液提取,采用Watses PRIME HLB固相萃取柱净化,通过BEH C18色谱柱分离,经0.1%甲酸水溶液-甲醇流动相系统梯度洗脱后,采用UPLC-MS/MS选择电喷雾ESI正离子模式多反应监测模式分析测定,基质添加标准曲线外标法定量。结果显示:硝基咪唑类及其代谢物标准曲线相关系数均≥0.9993,检出限为0.123~0.266μg·kg-1,回收率为85.7%~106.2%,相对标准偏差为3.2%~8.9%。说明该方法简便、快速、准确,可应用于水产品中硝基咪唑类及其代谢物残留的快速准确筛查和检测。
In order to detect nitroimidazoles and their metabolite residues,a method for determination of metronidazole,demenidazole,lornidazole,hydroxymetronidazole,hydroxymethyl metronidazole in aquatic products by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)was established.The samples were extracted with acetonitrile aqueous solution containing 0.2%formic acid,the residue contents were separated by BEH C18 chromatographic column,and eluted by 0.1%formic acid-methanol mobile phase systems,then analyzed by UPLC-MS/MS positive ion mode in multiple reaction monitoring modes.The quantitative information was obtained by matrix-added calibration with external standard.The correlation coefficient of calibration curves of tetracycline residues were above 0.9993.The limits of detection were 0.123-0.266μg·kg-1,the recovery rates of the method were 85.7%-106.2%,and the relative standard deviations(RSD)were 3.2%-8.9%.The method was simple,rapid and accurate,and would be used for the determination of nitroimidazoles and their metabolite residues residues in aquatic products.
作者
徐媛原
张微
张杨
李凯华
朱颖
肖曼
吴丹
张兵
XU Yuanyuan;ZHANG Wei;ZHANG Yang;LI Kaihua;ZHU Ying;XIAO Man;WU Dan;ZHANG Bing(Shenzhen Institute of Quality&Safety Inspection and Research,Shenzhen 518055,Guangdong China;Administration for Market Regulation of Guangdong Province Key Laboratory of Supervision for Edible Agricultural Praducts,Shenzhen 518055,Guangdong China)
出处
《饲料博览》
CAS
2022年第5期59-63,共5页
Feed Review
关键词
水产品
硝基咪唑
超高效液相色谱-串联质谱
aquatic product
nitroimidazole
ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)
作者简介
徐媛原(1991-),女,内蒙古赤峰人,硕士,工程师,研究方向为食用农产品质量安全检测与分析;通信作者:张兵(1972-),男,湖北荆州人,博士,高级农艺师,研究方向为食用农产品质量安全检测与分析。
