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
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。
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.
标题：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
英文标题：Simultaneous determination of sulfadiazine and trimethoprim residues in chicken fat by high performance liquid chromatography-tandem mass spectrometry
作者：
李文辉 北京市兽药监察所
李建 国家粮食和物资储备局科学研究院
孙志文 北京市兽药监察所
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,
发表日期：2019-11-19
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