鱼、虾中硝基呋喃代谢物和恩诺沙星残留联检技术研究

Simultaneous Determination of Nitrofuran Metabolites and Enrofloxacin Residues in Fish and Shrimp by High Performance Liquid Chromatography-tandemmass Spectrometry

建立了高效液相色谱-串联质谱法同时检测鱼、虾中硝基呋喃代谢物和恩诺沙星残留(恩诺沙星与环丙沙星之和)的检验方法。样品在超声波条件下快速衍生,用乙酸乙酯提取浓缩,并使用质谱电喷雾离子源,在正离子模式下测定,内标法定量。实验条件优化后,硝基呋喃代谢物和恩诺沙星残留量两类药物在1~50 ng/mL范围内有良好的线性关系>0.996;在2μg/kg、4μg/kg和20μg/kg的添加水平下,鱼的回收率和相对应的RSD分别为81.5%~93.0%、RSD≤9.07,109%~114%、RSD≤5.5,102%~112%、RSD≤5.01;虾的回收率和相对应的RSD分别为86.6%~99.5%、RSD≤5.69,94.1%~105%、RSD≤3.61,98.8%~108%、RSD≤5.08。该方法具有良好的精密度和准确度,能满足同步快速检验硝基呋喃代谢物和恩诺沙星残留量的需求。

To establish a coupled method for determination of nitrofuran metabolites and enrofloxacin residues in fish and shrimp by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The sample was quickly derivatized under ultrasonic condition,extracted and concentrated with ethyl acetate,and determined in positive ion mode using mass spectrometry electrospray ion source,and quantified by internal standard method.After optimizing the experimental conditions,there was a good linear relationship between nitrofuran metabolites and residual enrofloxacin in the range of 1~50 ng/mL,and the correlation coefficients were more than 0.996;At 3 spiked levels(2mg/kg,4mg/kg and 20mg/kg),the recoveries and RSD of fish were 81.5%~93.0%and RSD≤9.07,109%~114%and RSD≤5.5,102%~112%and RSD≤5.01,respectively;The recoveries and RSD of shrimp were 86.6%~99.5%and RSD≤5.69,94.1%~105%and RSD≤3.61,98.8%~108%and RSD≤5.08,respectively.The method which is applicable applicable for synchronous screening of nitrofuran metabolites and enrofloxacin residues in fish and shrimp,could meet the requirements for residue analysis on accuracy and precision.