A method for the determination of 4-aminoazobenzene in leather and fur was developed by using GC/MS and RRLC/DAD. Leather and fur samples were reduced by aqueous sodium dithionite solution in alkaline medium. The product of 4-aminoazobenzene was extracted with t-butylmethylether in the presence of sodium chloride. The qualitative and quantitative analysis of 4-aminoazobenzene were carried out by GC/MS and RRLC/DAD by comparing retention time and specific fragment ions. Pretreatment procedure of samples was optimized simply. Dyestuffs such as Disperse Yellow 23 and Disperse Orange 149 were used to evaluate applicability of this method. The proposed method iwas convenient and accurate with the recovery rate 79.8% ~104.0% , and it can be applied in 4 -aminoazobenzene analysis in leather and fur.% 建立了皮革和毛皮中4-氨基偶氮苯气相色谱质谱联用仪(GC/MS)和快速高分离度液相色谱/二极管阵列检测器(RRLC/DAD)的测定方法.样品在碱性介质中用连二亚硫酸钠还原，在氯化钠的存在下用叔丁基甲醚进行萃取，通过GC/MS的保留时间及特征离子并结合RRLC/DAD的数据进行定性和定量分析.对皮革和毛皮样品的前处理方法及基质对实验结果的影响进行了简单探讨，利用分散黄23和分散橙149对方法进行适用性评价.方法简便准确，加标回收率在79.8%耀104.0%，可用于皮革和毛皮中4-氨基偶氮苯的分析.
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