液相色谱-串联质谱法检测蜂蜜中15种喹诺酮类和17种磺胺类药物残留

Simultaneous determination of 15 kinds of quinolone residues and17 kinds of sulfonamide residues in honey by liquid chromatography-tandem mass spectrometry

中文关键词:  蜂蜜  液相色谱-串联质谱法  喹诺酮  磺胺

英文关键词:honey  liquid chromatography-tandem mass spectrometry  quinolones  sulfonamides

中文摘要:

      目的 建立同时测定蜂蜜中15种喹诺酮和17种磺胺类药物残留的液相色谱-串联质谱(liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)检测方法。方法 样品经过磷酸盐缓冲溶液(pH=8)提取, 过HLB(hydrophile-lipophile balance)固相萃取柱净化。以CORTECS C18色谱柱(2.1 mm×100 mm, 1.6 μm)分离, 以5 mmol乙酸铵、0.1%甲酸水(A)和0.1%甲酸-乙腈(B)作为流动相进行梯度洗脱。质谱分析以电喷雾为离子源(electrospray ionization, ESI+), 采用多反应监测(multiple reaction monitoring, MRM)。结果 本方法在15 min内完成32种目标化合物的分离。15种喹诺酮和17种磺胺类药物在1.0、5.0和10.0 μg/kg添加水平的回收率为54.9%~122.5%, 相对标准偏差(relative standard deviation, RSD)小于18.7%(n=6), 方法检出限为0.4 μg/kg, 定量限为1.0 μg/kg。结论 该方法快速、准确、灵敏, 适合测定蜂蜜中喹诺酮和磺胺类药物残留。

英文摘要:

      Objective To establish a method for the simultaneous determination of 15 kinds of quinolone residues and 17 kinds of sulfonamide residues in honey by liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The honey samples were diluted by phosphate buffer solution (PH=8) followed by a further cleanup procedure with Oasis (HLB) SPE column, and were eluted by gradient of 5 mmol ammonium acetate, 0.1% formic acid (A) and 0.1% formic acid-acetonitrile (B) as the mobile phase, separated by CORTECS C18 column (2.1 mm×100 mm, 1.6 μm). Mass spectrometry (MS) was used as ion source (ESI+) and multi-response monitoring (MRM). Results The separation of 32 target compounds were completed in 15 min. The recoveries of 15 kinds of quinolone residues and 17 kinds of sulfonamide residues at the levels of 1.0, 5.0 and 10.0 μg/kg were 54.9%~122.5% and the relative standard deviations (RSDs) were less than 18.7% (n=6). The limit of detection was 0.4 μg/kg, and the limit of quantification was 1.0 μg/kg. Conclusion The established method is rapid, accurate and sensitive, which is suitable for the determination of quinolone and sulfonamide residues in honey.