QuEChERS-超高效液相色谱-串联质谱法同时测定蜂蜜中21种磺胺类药物残留

Simultaneous determination of twenty-one sulfonamides residues in honey by QuEChERS ultra liquid chromatography-mass mass spectrometry

建立了同时测定蜂蜜中21种磺胺类药物残留的超高效液相色谱-串联质谱的测定方法。方法以氘代标准品为内标,样品以缓冲溶液(pH=4.00)溶解,1%甲酸乙腈提取,经盐析,胺丙基键合硅胶(NH2)吸附剂分散固相萃取净化后,采用超高效液相色谱-串联质谱选择反应监测正离子模式测定。方法的检出限为0.12~2.46μg/kg,标准溶液在0.05~60 ng/m L内具有良好线性,相关系数均大于0.99,平均回收率为60.44%~107.80%。方法简单、快速、稳定、准确、灵敏度高,适合于实验室大批量样品检测。

The method for simultaneous determination of 21 sulfonamide residues in honey was developed by Ultra high performance liquid chromatography-tandem mass spectrometry（UPLC-MS/MS）. Deuterium substituted standards were used as internal standards and added to the sample before extraction. The sample was dissolved by buffer solution（pH = 4. 00）,extracted with 1% formic acid in acetonitrile,purified by salting-out and cleaned up by NH2 adsorbent. The mass spectrometer was operated in the positive ion mode using multiple-reaction monitoring for qualitative and quantization. The detection limit of the method was 0. 12-2. 46 μg/kg. The correlation coeficient of linear calibration curve was over 0. 99 within the range of sulfonamides concentration 0. 05-60 ng/m L. The average recoveries for 21 sulfonamide residues were 60. 44%-107. 80%. The method is simple、rapid、reliable、stable and sensitive. It＇s suitable for high throughout determination of 21 sulfonamide residues in honey.