HPLC-MS/MS法测定鱼肉中19种喹诺酮类抗生素的残留研究

Simultaneous Determination of 19 Quinolone Antibiotics Residues in Fish by HPLC-MS/MS

建立了鱼肉中麻保沙星、吡哌酸、培氟沙星、氧氟沙星、诺氟沙星、依诺沙星、恩诺沙星、环丙沙星、洛美沙星、单诺沙星、沙拉沙星、二氟沙星、奥索利酸、西诺沙星、氟甲喹、萘啶酸、奥比沙星、氟罗沙星和司帕沙星共19种喹诺酮类(QNs)抗生素的高效液相色谱串联质谱(High Performance Liquid Chromatography Tandem Mass Spectrometry,HPLC-MS/MS)检测分析方法。鱼肉加入LEDTA-Macllvaine缓冲溶液后经酸化乙腈萃取,用一定配比的甲醇和0.1%的甲酸水溶液作流动相,梯度洗脱,HPLC-MS/MS采用电喷雾正离子(ESI+)电离,配合多反应监测模式分析,采用添加标准物质外标法定量分析。结果发现,19种QNs抗生素在1~200μg·L^(-1)具有良好的线性关系,相关系数不低于0.9980;添加3组不同浓度的混标,加标回收率在69.23%~96.28%,相对标准偏差在6.28%~9.86%。该方法具有分析时间短、操作简单、定性准确高及检出限低等优点,满足残留分析的要求。

A high performance liquid chromatography tandem mass spectrometry(HPLC-MS/MS)method was established for the detection and analysis of 19 quinolones(QNs)in fish meat,including maprofloxacin,pipemidic acid,pefloxacin,ofloxacin,norfloxacin,enoxacin,enrofloxacin,ciprofloxacin,lomefloxacin,monofloxacin,salafloxacin,difloxacin,oxalic acid,cinofloxacin,flemequine,naridinic acid,obifloxacin,fleroxacin and sparfloxacin.Fish meat is extracted with acidified acetonitrile after adding ledta macllvaine buffer solution.Methanol and 0.1%formic acid aqueous solution are used as mobile phase for gradient elution.HPLC-MS/MS adopts electrospray positive ion(ESI+)ionization and multi reaction monitoring mode analysis.Quantitative analysis is performed by adding standard substance external standard method.The 19 QNs antibiotics showed a good linear relationship in the range of 1~200μg·L^(-1) and the correlation coefficient was not less than 0.9980;three groups of mixed standards with different concentrations were added.The recoveries were 69.23%~96.28%,and the relative standard deviations were 6.28%~9.86%.This method has the advantages of short analysis time,simple operation,high qualitative accuracy and low detection limit,and meets the requirements of residue analysis.