高效液相色谱-串联质谱法测定鸡蛋中9种禁用药物残留方法的建立

Establishment of a High Performance Liquid Chromatography-tandem Mass Spectrometry Method for the Determination of 9 Prohibited Drugs in Eggs

为有效检测鸡蛋中甲硝唑、诺氟沙星、强力霉素、氧氟沙星、培氟沙星、金刚烷胺、恩诺沙星、氟苯尼考、氯霉素9种药物残留,建立高效液相色谱-串联质谱(HPLC-MS/MS)分析方法,对方法中的提取液、仪器条件等进行优化;设计试验方案,考察方法的回收率、灵敏度及精密度。鸡蛋样品去壳混匀后用80%乙腈水溶液提取,PRiME HLB小柱净化,洗脱液经氮气吹干后用10%甲醇水溶液复溶,经0.22μm微孔滤膜过滤后,用高效液相色谱-串联质谱仪测定。分析方法采用电喷雾电离正负离子同时进行扫描,多反应监测(MRM)模式进行测定。在4个不同浓度的水平下,平均回收率在75.7%~95.7%;相对标准偏差(RSD)均小于10%;检测限(LOD,S/N>3)和定量限(LOQ,S/N>10)分别为1.0μg/kg和2.0μg/kg。本检测方法简便快捷,精确灵敏,稳定可靠,适用于对鸡蛋中多种药物残留的快速检测和分析。

To establish an efficient method for the detection of metronidazole,norfloxacin,doxycycline,ofloxacin,pefloxacin,amantadine,enrofloxacin,florfenicol and chloramphenicol in eggs using high performance liquid chromatographytandem mass spectrometry(HPLC-MS/MS).After establishing the basic method,the extraction liquid and instrument conditions in the method were optimized;the experimental scheme was designed to investigate the method recovery rate,sensitivity and precision.Egg samples were extracted with 80%acetonitrile aqueous solution and purified with a PRiME HLB cartridge.The purified solution was blown dry with nitrogen and dissolved with 10%methanol in water.After 0.22μm micro porous membrane filtration,it was subjected to high performance liquid chromatography-tandem mass spectrometry.Simultaneous scanning with electrospray ionization of positive and negative modes,multiple reaction monitoring(MRM)mode determination.At 4 different concentration levels,the average recovery was 75.7%to 95.7%;the relative standard deviation RSD was less than 10%;the limit of detection(LOD,S/N>3)and limit of quantification(LOQ,S/N>10)are 1.0μg/kg and 2.0μg/kg respectively.The method is simple,fast,accurate,sensitive,stable and reliable,and is suitable for rapid detection and analysis of various drug residues in eggs.