液相色谱-串联质谱负离子模式测定鸡肉中磺胺硝苯的残留  

Determination of Sulfanitran Residue in Chicken by Liquid Chromatography-Tandem Mass Spectrometry with Negative Ion Mode

作　　者：魏云计[1] 朱臻怡[1] 冯民[1] 王小晋[1] 何健[1] 张伶俐[1] 魏斌[1] 丁涛[2] 

机构地区：[1]淮安出入境检验检疫局,江苏淮安223001 [2]江苏出入境检验检疫局动植物与食品检测中心,江苏南京210001

出　　处：《肉类研究》2016年第8期35-38,共4页Meat Research

基　　金：质检总局科技计划基础研究类项目(2015IK132)

摘　　要：建立高效液相色谱-串联质谱测定鸡肉中磺胺硝苯残留的方法。样品经过甲酸-乙酸乙酯（2∶98,V/V）提取,正己烷脱脂,液-液分配净化后,C18柱分离,甲醇、5 mmol/L乙酸铵为流动相梯度洗脱,采用负离子扫描多反应监测（multiple reaction monitoring,MRM）模式下液质联用仪进行定性和定量分析。在2.0-100.0μg/L质量浓度范围内,线性相关系数大于0.99,方法的检出限和定量限分别为0.5μg/kg和2.0μg/kg,在2.0、5.0、10.0μg/kg添加量的回收率为76.0%~83.4%,相对标准偏差（relative standard deviation,RSD）小于8.7%。该方法简便快捷,可用于鸡肉中磺胺硝苯残留量测定。A method for the determination of sulfanitran in chicken was developed by liquid chromatography-tandem mass spectrometry. Samples were extracted with formic acid-ethyl acetate（2：98, V/V）, and the extract was defatted by hexane extraction and cleaned up by liquid-liquid partitioning. The analyte was separated on a C18 colum using a mobile phase consisting of methanol and 5 mmol/L ammonium acetate solution with gradient elution. The mass spectrometry was operated in negative ion mode using multiple reaction monitoring（MRM） for qualitative and quantitative analysis. The calibration curve of the method was linear in the range of 2.0–100.0 μg/L, with correlation coefficient more than 0.99. The limit of detection（LOD） and limit of quantitation（LOQ） were 0.5 μg/kg and 2.0 μg/kg, respectively. At spiked levels of 2.0, 5.0, 10.0 μg/kg, the recoveries ranged from 76.0% to 83.4% with relative standard deviations（RSD） less than 8.7%. This method proved to be convenient and suitable for the determination of sulfanitran residues in chicken.

关 键 词：液相色谱-串联质谱 负离子模式 鸡肉 磺胺硝苯 

分 类 号：TS251.7[轻工技术与工程—农产品加工及贮藏工程] O657.63[轻工技术与工程—食品科学与工程]