柱前衍生HPLC法检测罗非鱼肌肉中的硫酸新霉素  

Determination of Neomycin sulfate in Tilapia muscle by high performance liquid chromatography with pre-column derivatization

作　　者：宋洁[1,2] 王伟利[1] 姜兰[1] 王贤玉[1] 

机构地区：[1]中国水产科学研究院珠江水产研究所,广东广州510380 [2]上海海洋大学水产与生命学院,上海201306

出　　处：《广东农业科学》2011年第3期142-143,147,共3页Guangdong Agricultural Sciences

基　　金：国家"十一五"科技支撑计划项目(12006BAD03B04-02);广东省农业攻关项目(2008A020100006)

摘　　要：硫酸新霉素本身没有紫外吸收,必须通过柱前衍生来进行荧光检测,建立合适的衍生方法是提高检测灵敏度的关键。通过对硫酸新霉素衍生方法的优化,确定衍生化学试剂氯甲酸戊甲酯乙腈溶液的浓度为8 mmol/L,在pH值为7.8的硼酸缓冲液中衍生反应15 min,10 h内检测可得到理想的结果。对硫酸新霉素检测方法优化后,该药物在罗非鱼肌肉中检测限可达到0.02mg/kg,定量限为0.05 mg/kg,在0.05~5 mg/kg浓度范围内有良好的线性关系（r2=0.9956）,在肌肉中分别按照0.10、0.50、1.00 mg/kg的标准添加硫酸新霉素,回收率分别为76.43±1.46%、79.47±1.71%、86.82±1.13%。Neomycin sulfate has no UV absorption and the fluorescence detection have to use pre-column derivatization.Establish a appropriate derivatization method is crucial to improve the detection sensitivity.Optimal conditions for the derivatization of neomycin sulfate was described,the concentration of 9-fluorenylmethyl chloroformate in acetonitrile solution was 8 mmol/L,the reaction is 15 min in pH=7.8 of borate buffer,the derivative was detected in 10 h.The determination of Neomycin sulfate was optimized,the detection limits of neomycin sulfate in Tilapia mascle was 0.02 mg/kg,the limit of quatification was 0.05 mg/kg,The detection had a good linearity（r2=0.9956,n=6）in the range of 0.05~5 mg/kg,The recovery were 76.43±1.46%、79.47±1.71%、86.82±1.13% respectively at the concentration of 0.10,0.50,1.00 mg/kg.

关 键 词：罗非鱼 硫酸新霉素 高效液相色谱法 氯甲酸芴甲酯 柱前衍生化 

分 类 号：X503.225[环境科学与工程—环境工程]