高效液相色谱串联质谱法测定鸡肉组织中氨苯砜残留的研究  

Determination of Dapsone in Chicken Muscle Tissues by High Performance Liquid Chromatography Tandem Mass Spectrometry

作　　者：彭涛[1] 谢洁[1,2] 陈冬东[1] 王娉[1] 王旗[2] 裴星瑶 谢三磊[2] 范春林[1] 江海洋[2] 

机构地区：[1]中国检验检疫科学研究院,北京100176 [2]中国农业大学动物医学院,北京100193

出　　处：《中国家禽》2015年第17期23-26,共4页China Poultry

基　　金：国家科技支撑计划(2013BAD18B11、2012BAD33B02、2012BAK08B01);公益性行业(农业)科研专项(201203040)

摘　　要：研究建立了检测鸡肉组织中氨苯砜的高效液相色谱串联质谱（HPLC-MS/MS）定量确证方法。样品采用1%乙酸-乙腈（v/v）提取,乙腈饱和正己烷脱脂,采用C18反相色谱柱分离,以乙腈和5 mmol/L乙酸铵水溶液（含0.1%甲酸）为流动相,梯度洗脱,电喷雾电离,正离子-多反应监测扫描模式,氨苯砜的定量、定性离子分别为249.1〉156.0,249.1〉108.0。建立的方法在0.05-10μg/kg范围内线性良好,检测限为0.015μg/kg,定量限为0.05μg/kg,在0.05-5μg/kg的添加范围内,回收率在76.2%-94.5%之间,日内、日间变异系数均小于19.4%。Abstract：In this study,a high performance liquid chromatography tandem mass spectrometry （HPLC-MS/MS）method was developed for the determination of dapsone in chicken muscle tissues. The samples were extracted with acidic acetonitrile and defatted by hexane. Chromatographic separation was performed on a C1s column using acetonitrile and 5 mmol/L ammonium acetate （containing 0.1% formic acid）in positive mode. The targets were analyzed by HPLC-MS/MS with electro-spray ionization interface in multiple reaction monitoring mode. The quantitative and qualitative ion pair were 249.1〉156.0 and 249.1〉108.0, respectively. The externally matrix-matched calibration curves were prepared on each validation day to give 5-point calibration curves ranging from 0.05 to 10 μg/kg. The limits of detection and limits of quantification were 0.015 μg/kg and 0.05 μg/kg, respectively. The recoveries in chicken muscles were 76.2% to 94.5% at fortified levels of 0.05 to 5 μg/kg. The repeatability and within-laboratory reproducibility were not more than 19.4%.

关 键 词：HPLC-MS/MS 氨苯砜 鸡肉组织 检测 

分 类 号：S859[农业科学—临床兽医学]