同时检测淡水鱼加工中土霉素和微囊藻毒素(MC-LR)残留量

Simultaneous Determination of Oxytetracycline and Microcystin-LR Residues in Freshwater Fish Products

目的：土霉素是限制我国淡水鱼深加工产品出口的关键抗生素之一；此外，由于水污染加重，淡水鱼中藻毒素残留问题也很严重。研究和开发同时快速检测技术已成为当前急需解决的问题。方法：鲫鱼鱼肉进行不同前处理，利用高效液相色谱测定毒素残留量。结果：土霉素和微囊藻毒素的最低检测限分别为0．1μg/kg、5ng/L,。质量浓度范围0．1～5．Oμg/mL的土霉素、微囊藻毒素标准品制备标准曲线，线性关系较好，相关系数分别为0．995、0．998。精密度分别为1．82％、1．68％；回收率范围分~t188．1％～102．8％、90．6％～105％。结论：对比酶联免疫反应试剂盒的检测，2种方法结果没有太大差别。

A rapid HPLC method for simultaneous determination of oxytetracycline and microcystin-LR （MC-LR） residues in freshwater fish products has been proposed. Five different sample pretreatment methods were compared. The limit of detection was 0.1 μg/kg for oxytetracycline and 5 ng/L for microcystin-LR. Calibration curves for both analytes were linear in the range between 0.1 and 5.0 μg/mL and the correlation coefficients were 0.995 and 0.998, respectively. The precision, expressed as relative standard deviation （RSD）, was 1.82% for oxytetracycline and 1.68% for microcystin-LR, and the recoveries from spiked crucian carp muscle samples ranged from 88.1% to 102.8% for oxytetracycline and from 90.6% to 105% for MC-LR. The analytical results from the HPLC method were very similar to those obtained with an ELISA assay kit.