鸡皮脂组织中尼卡巴嗪残留量的测定高效液相色谱-串联质谱法  

DETERMINATION OF NICARBAZIN RESIDUE IN CHICKEN SKIN/FAT HIGH PERFORMANCE LIQUID CHROMATOGRAPHY-TANDEM MASS SPECTROMETRY

作　　者：侯婷 王霄旸[1] 张丽芳[1] 张可煜[1] 薛飞群[1] HOU Ting;WANG Xiao-yang;ZHANG Li-fang;ZHANG Ke-yu;XUE Fei-qun(Key Laboratory of Veterinary Chemical Drug and Pharmaceutics,Ministry of Agriculture,Shanghai Veterinary Research Institute,CAAS,Shanghai200241,China)

机构地区：[1]中国农业科学院上海兽医研究所农业部兽用化学药物及制剂学重点实验室,上海200241

出　　处：《中国动物传染病学报》2018年第2期74-79,共6页Chinese Journal of Animal Infectious Diseases

基　　金：公益性行业(农业)科研专项经费(201303038);国家青年自然基金(31602113);国家科技支撑计划-新型动物专用化学药物的创制及产业化关键技术研究(2015BAD11B01)

摘　　要：本研究旨在建立一种检测鸡皮脂组织中尼卡巴嗪标志物4,4-二硝基均二苯脲残留量的高效液相色谱-串联质谱法。组织样品用乙腈提取,氮气吹干浓缩,正己烷除脂、甲醇水溶液(75∶25,v/v)萃取,高效液相色谱-串联质谱法测定,内标法定量。该方法在50~1000 ng/m L范围内,线性关系良好,线性相关系数r=0.9998,该方法的检测限和定量限分别为2.5μg/kg和25μg/kg,加标平均回收率为98.10%~114.11%,批内批间的RSDs均小于5%,具有较好的回收率和重复性。该方法简单、快速、有效,可用于鸡皮脂中尼卡巴嗪残留标志物残留量的定量检测。The aim of the study was to establish a method for determing 4,4-dinitrocarbanilide residual,the residual marker of Nicarbazin in chicken skin/fat.The sample was extracted by acetonitrile,and concentrated by nitrogen.In the extractive,the fat layer was removed by hexane,the target object was extracted by methanol-water solution(75∶25,v/v),then the sample was measured by High performance liquid chromatography-tandem mass spectrometry,and quantifi ed with internal standard method.The method showed good lineatity in the range of 50~1000 ng/mL with correlation coeffi cients(r)was 0.9998.The limit of detection(LOD)and the limit of quantitation(LOQ)of the method were 2.5μg/kg and 25μg/kg,respectively.The average recoveries of spiked samples were between 98.10%and 114.11%,and the relative standard deviations(RSDs)in intra-batch and inter-batch were below 5%,having good recoveries and repeatabilitys.This method was simple,rapid,effective and suitable for detecting the residual markers of Nicarbazin residue in chicken skin/fat.

关 键 词：鸡皮脂组织 尼卡巴嗪 4 4-二硝基均二苯脲(DNC) 高效液相色谱-串联质谱法(HPLC-MS/MS) 

分 类 号：S859.795[农业科学—临床兽医学]