高效液相色谱-串联质谱法同时测定鸡脂肪中磺胺嘧啶、甲氧苄啶的残留量

Simultaneous determination of sulfadiazine and trimethoprim residues in chicken fat by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  鸡脂肪  磺胺嘧啶  甲氧苄啶  高效液相色谱-串联质谱法

英文关键词:chicken fat  sulfadiamine  methoxil  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)同时测定鸡脂肪中磺胺嘧啶、甲氧苄啶的残留量的方法。方法 样品经乙腈2次提取, 以乙腈和0.1%甲酸水溶液为流动相进行溶解后, 用正己烷2次脱脂, 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。结果 0.5~100 ng/mL的浓度范围内磺胺嘧啶、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; 鸡脂肪样品中磺胺嘧啶、甲氧苄啶在1.0~200.0 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%。结论 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。

英文摘要:

      Objective To establish a method for simultaneous determination of sulfadiazine and trimethoprim residues in chicken fat by high performance liquid chromatography-tandem mass spectrometry. Methods 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. Results In the concentration range of 0.5?100 ng/mL, the chromatographic peak area of sulfadiazine and trimethoprim showed a good linear correlation with the concentration, and the correlation coefficients were all greater than 0.99 and limit of quantity was 1.0 μg/kg. The average recoveries of sulfadiazine and trimethoprim in chicken fat samples at the addition level of 1.0 to 200.0 μg/kg were 66.3%?97.5%, and the relative standard deviations within the batch and between batches were less than 20%. Conclusion 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.