液相色谱-串联质谱法同时测定蜂蜜中17种 磺胺类药物的残留量

Simultaneous determination of 17 kinds of sulfonamides in honey by liquid chromatography-tandem mass spectrometry

中文关键词:  磺胺类药物  液相色谱-串联质谱法  固相萃取  蜂蜜

英文关键词:sulfonamides  liquid chromatography-tandem mass spectrometry  solid phase extraction  honey

中文摘要:

      目的 建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry, LC-MS/MS)同时测定蜂蜜中的17种磺胺类药物。方法 蜂蜜样品经0.1 mol/L盐酸溶液溶解, 经正己烷除脂、固相萃取柱净化, 采用CAPCELL PAK C18色谱柱分离; 质谱采用电喷雾正离子电离模式(electrospray ionization, ESI+)和多反应扫描监测模式(multi reaction monitoring, MRM)进行测定, 以内标法定量。结果 17种磺胺类药物的检出限为0.1~1.0 μg/kg; 在0.5~50 μg/kg范围内线性关系良好, 相关系数r>0.99; 回收率在82.40~100.6%之间, 相对标准偏差为1.0~6.0%(n=6)。结论 本方法灵敏度高、准确性好, 可适用于蜂蜜中多种磺胺类药物残留的检测。

英文摘要:

      Objective To establish a method for the simultaneous determination of 17 kinds of sulfonamides in honey by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Methods Honey was dissolved with 0.1 mol/L hydrochloric acid, removed fat with n-hexane and cleaned up with solid phase extraction column, and then separated by CAPCELL PAK C18 column. Mass used electrospray ionization positive ionization mode (ESI+) and multiple reaction monitoring (MRM) for determination with internal standard method for quantification. Results The limits of detection of 17 kinds of sulfonamides were 0.1~1.0 μg/kg. The method showed a good linearity over the range of 0.5~50 μg/kg with r>0.99. The average recoveries were in the range of 82.40~100.6%, while the relative standard deviations (RSD) were 1.0~6.0%(n=6). Conclusion The established method is highly sensitive and accurate, which is suitable for the detection of sulfonamides in honey.