超高效液相色谱-串联质谱法同时检测鸡蛋中5种磺胺类药物和甲氧苄啶残留量

Simultaneous Determination of Five Sulfonamide and Trimethoprim Residues in Eggs by Ultrahigh-performance Liquid Chromatography-tandem Mass Spectrometry

关键词:  鸡蛋  磺胺类药物  甲氧苄啶  液相色谱-串联质谱法

Key words:  egg  sulfonamide  trimethoprim  high performance liquid chromatography-tandem mass

摘要:

建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时测定鸡蛋中5种磺胺类药物和甲氧苄啶的残留量的方法。样品经乙腈提取2次, 以乙腈和0.1%甲酸水溶液为流动相进行溶解后, 用正己烷脱脂2次, 过滤膜后用于液相色谱串联质谱仪测定, 基质添加标准溶液外标法定量。0.5~100 ng/mL的浓度范围内5种磺胺类药物和甲氧苄啶色谱峰面积与浓度呈良好线性相关, 相关系数均大于0.99; 方法定量限为1.0 μg/kg; 鸡蛋样品中5种磺胺类药物和甲氧苄啶在1.0~100.0 μg/kg添加水平内的平均回收率在66.3%~97.5%之间, 批内批间相对标准偏差均小于20%。该方法回收率满足残留检测要求, 且方法的重现性良好, 满足国内外兽药残留相关法规规定。

Abstract:

To establish a method for simultaneous determination of five kinds of sulfonamide and trimethoprim residues in eggs by high performance liquid chromatography-tandem mass spectrometry. Samples were extracted twice with acetonitrile, dissolved in acetonitrile and 0.1% formic acid aqueous solution as mobile phases, degreased twice with n-hexane, filtered through a membrane and used for determination by liquid chromatography tandem mass spectrometry, and quantified by external standard method with matrix addition. In the concentration range of 0.5?100 ng/mL, the chromatographic peak area of five kinds of sulfonamide and trimethoprim showed a good linear correlation with the concentration, and the correlation coefficients were all greater than 0.99. The average recovery of five kinds of sulfonamide and trimethoprim in egg samples at the addition level of 1.0 to 100.0 μg/kg were 66.3%?97.5%, and the relative standard deviations within the batch were less than 20%. The recovery rate of this method meets the requirements for residue detection, and this method has good reproducibility, which meets the relevant domestic and foreign veterinary drug residue regulations.