液质联用法测定鸡肉组织中氯霉素残留的研究  

Study on HPLC/MS-MS analysis of chloramphenicol in chicken tissue

作　　者：陈小霞[1] 岳振峰[2] 郑卫平[2] 谢丽琪[2] 梁世中[3] 

机构地区：[1]深圳大学教务处,深圳518060 [2]深圳出入境检验检疫局食品检验检疫技术中心,深圳518067 [3]华南理工大学生物科学与工程学院,广州510640

出　　处：《药物分析杂志》2006年第1期110-113,共4页Chinese Journal of Pharmaceutical Analysis

基　　金：国家质量监督检验检疫总局科技项目(项目编号:2003IK047)

摘　　要：目的:建立鸡肉中氯霉素残留的电喷雾电离液质联用(LC/ESI-MS-MS)定性定量检测方法。方法:选用 Agilent Zorb-ax BDS C_(18)(2.1mm×150mm,3.5μm)反相色谱柱,以乙酸乙酯为提取溶剂,流动相为乙腈-水(起始比例90:10,梯度洗脱),进样量30μL,流速0.3mL·min^(-1),采用大气压喷雾电离源液质联用仪测定,定量离子 m/z 152.1(负离子),监测模式为多反应监测(MRM)。结果:方法的检出限为0.01μg·kg^(-1),测定低限为0.10μg·kg^(-1),线性范围为0.05～1.00μg·L^(-1),加标回收率为74.3%～84.0%,RSD 为7.9%～12.3%。结论:该方法灵敏、准确、简便、快速,能够满足残留检测的要求。Objective： To develop an HPLC/ESI - MS - MS method for determination and confirmation of chloramphenicol residue in chicken tissue. Method：Use Agilent Zorbax Clscolumn（2. 1 mm ×150 mm,3.5 μm） ;Extract samples with ethyl acetate ; Mobile phase is acetonitfile -water（ initial proportion 90： 10, gradient） ;Injection volume is 30 μL;Flow rate is O. 3 mL · min^-1 ;The mass spectrometer is equipped with ESI source and operated in the negative ion mode using multiple reaction monitoring,and the quantitation ion is m/z 152. 1. Results：The limit of detection（LOD） was 0. 01 μg ·kg^-1, and the limit of quantitation （LOQ）was 0O. 10 μg · kg^-1. The linear plots were obtained between O. 050 and 1. 00 μg · L^-1. Overall recoveries were between 74. 3% and 84. 0% with RSD values between 7.9% and 12. 3 %. Conclusion： The method is sensitive, accurate, convenient and fast, which can meet the requirements for residue determination.

关 键 词：液质联用仪 氯霉素 残留 测定 

分 类 号：R917[医药卫生—药物分析学]