高效液相色谱-串联质谱法同时测定水产品中诺氟沙星、环丙沙星和恩诺沙星

Simultaneous determination of norfloxacin,ciprofloxacin and enrofloxacin residues in aquatic products by high performance liquid chromatography-tandem mass spectrometry

建立了一种同时测定水产品中诺氟沙星、环丙沙星与恩诺沙星药物残留的高效液相色谱-串联质谱（HPLCMS/MS）方法。样品经乙腈提取,用正己烷脱脂,旋转蒸发浓缩,采用HPLC-MS/MS选择反应监测（SRM）正离子模式测定进行定性和定量分析。结果表明,诺氟沙星、环丙沙星与恩诺沙星药物检测结果的检出限（LOD）为1.0μg/kg,定量限（LOQ）为2.0μg/kg,检测结果的相对标准偏差为1.8%~10.9%（n=6）,加标回收率达到68.5%~102.1%。该方法具有重现性好、灵敏度高、分析时间短和确证能力强等优点,适用于水产品中诺氟沙星、环丙沙星与恩诺沙星药物残留的确证检测。

An analytical method for the simultaneous determination of norfloxacin,ciprofloxacin and enrofloxacin resi- dues in aquatic products by high performance liquid chromatography- tandem mass spectrometry（ HPLC- MS / MS） was established. The sample was extracted with acetonitrile,cleaned- up by hexane,and concentrated with a rotary evaporator. The mass spectrometer was operated in the positive ion mode using selected reaction monitoring for the qualitative and quantitative analysis. The detection limits of this method for norfloxacin,ciprofloxacin and enrofloxacin residues were 1. 0 μg / kg,and the limits of quantification were 2. 0 μg / kg. The relative standard deviations ranged from 1. 8% to 10. 9%（ n = 6） and the recovery rates were from 68. 5% to 102. 1%. The method was proved to have good repeatability and high sensitivity,and be rapid,reliable and suitable for the simultaneous determination of nor- floxacin,ciprofloxacin and enrofloxacin residues in aquatic products.