超高效液相色谱-质谱串联法测定蜂蜜中喹诺酮类药物残留

Determination of quinolone residues in honey by ultra performance liquid chromatography-mass spectrometry

中文关键词:  蜂蜜  喹诺酮类  药物残留  超高效液相色谱-串联质谱法

英文关键词:honey  quinolones  drug residues  ultra performance liquid chromatography-mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-质谱串联法测定蜂蜜中喹诺酮类药物残留的分析方法。方法 分析采用Thermo Fisher Gold Hypersil柱(50 mm×2.1 mm, 1.9 μm); 流动相A为甲醇, 流动相B为0.1%甲酸水溶液, 流动相流速: 0.2 mL/min, 柱温: 35 ℃, 梯度洗脱; 电喷雾离子源正离子扫描 (electron spray ionization, ESI+), 选择反应监测模式检测(selected reaction monitoring, SRM)。结果 6种喹诺酮类药物在各自范围内线性关系良好, 相关系数r均大于0.998, 平均加样回收率在82.47%~105.06%, 相对标准偏差(relative standard deviation, RSD)均小于5.62%。12批次样品中有2批次检出诺氟沙星。结论 该方法前处理简单、快捷、测定灵敏度高、结果准确, 可适用于蜂蜜中喹诺酮类药物残留量的检测, 为监督检验提供了更为简单准确的方法。

英文摘要:

      Objective To establish a method for the determination of quinolones residues in honey by ultra performance liquid chromatography-mass spectrometry. Methods Thermo Fisher Gold Hypersil column (50 mm ×2.1 mm, 1.9 μm) was used for analysis. Mobile phase A was methanol, mobile phase B was 0.1% formic acid solution, mobile phase flow rate was 0.2 mL/min, column temperature was 35 ℃, and gradient elution was performed. The detection was electrospray ion source positive ion scan (ESI+) and the selective reaction monitoring mode detection (SRM). Results The 6 quinolone residues showed good linear relationships within their own ranges (r≥0.998). The average recoveries were 82.47%?105.06%, with the relative standard deviations were less than 5.62%. There were 2 out of 12 samples were detected norfloxacin. Conclusion This method is simple, rapid, sensitive, and accurate, which can be applied to detect quinolone residues in honey, and provides a simpler and more accurate method for supervision and inspection.