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目的建立高效液相色谱-串联质谱法测定鱼肉组织样品中16种(氟)喹诺酮类药物残留分析方法。方法样品经乙酸铵缓冲液-乙腈提取,正己烷脱脂净化后,用Atlantis C18柱分离,以乙腈水(含0.4%甲酸)作为流动相,采用电喷雾离子源(ESI),阳离子模式,多反应监测(MRM)方式检测,外标法定量。结果在以上实验条件下,16种(氟)喹诺酮类药物在0.020～5.0mg/L范围内线性良好,最低检出浓度0.50～31.4g/kg,相对标准偏差(RSD)在0.99%～5.94%之间,样品平均加标回收率在62.2%～99.2%之间。共检测鱼肉组织样品81份,检出的(氟)喹诺酮药物为培氟沙星、洛美沙星、环丙沙星和恩诺沙星,检出浓度在0.11×10-3～4.9×10-3mg/kg之间。结论该方法能同时定性及定量分析鱼肉组织样品中多种(氟)喹诺酮类药物残留,方法精密度较好,准确度较高,结果较满意。
OBJECTIVE To establish a method for the determination of 16 fluoroquinolones residues in fish tissue samples by high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with ammonium acetate buffer - acetonitrile, degreased with n-hexane, separated on an Atlantis C18 column, eluted with acetonitrile water (containing 0.4% formic acid) as mobile phase and electrospray ionization (ESI) Monitoring (MRM) method of detection, external standard quantitative. Results Under the above experimental conditions, the 16 fluoroquinolones showed good linearity in the range of 0.020-5.0 mg / L with the lowest detectable concentrations of 0.50-31.4 g / kg and the relative standard deviations (RSDs) of 0.99% -5.94% The average spike recoveries ranged from 62.2% to 99.2%. A total of 81 samples of fish tissues were detected. The detected fluoroquinolones were pefloxacin, lomefloxacin, ciprofloxacin and enrofloxacin. The detected concentrations were 0.11 × 10-3 ~ 4.9 × 10- 3mg / kg. Conclusion The method can qualitatively and quantitatively analyze the residues of fluoroquinolones in fish tissue samples. The method has good precision and high accuracy, and the results are satisfactory.