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/mL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2.5 μg /kg 和25 μg /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 quantified with internal standard method. The method showed good lineatity in the range of 50~1000 ng /mL with correlation coefficients(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.
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