高效液相色谱-串联质谱法测定预制菜中6种喹诺酮类抗生素和强力霉素残留量

Determination of 6 kinds of quinolones and doxycycline residues in prepared dishes by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  高效液相色谱串联质谱法  预制菜  抗生素  喹诺酮类  强力霉素

英文关键词:high performance liquid chromatography-tandem mass spectrometry  prepared dishes  antibiotics  quinolones  doxycycline

中文摘要:

      目的 建立高效液相色谱-串联质谱法同时测定预制菜中喹诺酮类抗生素(恩诺沙星、环丙沙星、诺氟沙星、培氟沙星、氧氟沙星、洛美沙星)和强力霉素残留量。方法 使用84%乙腈水溶液(1%冰乙酸)为提取溶液, 以Oasis Prime-HLB固相萃取柱净化富集, 收集全部流出液, 氮吹近干, 加入1 mL复溶液10%甲醇水溶液(含1%冰乙酸)涡旋溶解, 取上清过0.22 μm微孔滤膜, 经Waters ACQUITY UPLC TM BEH C18柱(100 mm×2.1 mm, 1.7 μm)分离, 以甲醇和0.1%甲酸水溶液为流动相, 电离方式为喷雾正离子模式, 采用多反应监测模式通过高效液相色谱-串联质谱仪进行分析。结果 7种抗生素在考察浓度范围内线性关系良好(r>0.9990), 方法检出限为0.03~0.24 μg/kg, 定量限为0.09~0.72 μg/kg, 加标回收率为84.5%~114.0%, 相对标准偏差为1.1%~4.1%。结论 本研究所建立的方法方便快捷、准确度高、稳定性好, 能够对预制菜中6种喹诺酮类兽药残留及强力霉素残留进行定量分析。

英文摘要:

      Objective To establish a method for the simultaneous determination of quinolones antibiotics (enrofloxacin, ciprofloxacin, norfloxacin, pefloxacin, ofloxacin, lomefloxacin) and doxycycline residues in prepared dishes by high performance liquid chromatography tandem mass spectrometry. Methods The 84% acetonitrile aqueous solution (1% ice acetic acid) was used as extraction solution, Oasis Prime-HLB solid phase extraction column was used to purify and concentrate, all the eluents were collected, nitrogen-blown to nearly dry, and 1 mL of complex solution 10% methanol aqueous solution (containing 1% ice acetic acid) was added to vortex dissolve, and 0.22 μm microporous filter membrane was taken as supernatant. The Waters ACQUITY UPLC TM BEH C18 column (100 mm×2.1 mm, 1.7 μm) was separated, methanol and 0.1% formic acid aqueous solution were used as mobile phase, ionization mode was spray positive ion mode, and the analysis was performed by high performance liquid chromatography tandem mass spectrometry using multiple reaction detection mode. Results The linear correlation of the 7 kinds of antibiotics was good (r>0.9990). The limits of detection were 0.03–0.24 μg/kg and the limits of quantitatation were 0.09–0.72 μg/kg. The recoveries were 84.5%–114.0% and the relative standard deviations were 1.1%–4.1%. Conclusion The method established in this study is convenient, rapid, accurate and stable, and can be used for quantitative analysis of 6 kinds of quinolone veterinary drug residues and doxycycline residues in prepared dishes.