高效液相色谱法检测罗非鱼中氯霉素的残留量

Determination of chloramphenicol residues in tilapia by high performance liquid chromatography

目的建立高效液相色谱法(high performance liquid chromatography,HPLC)测定罗非鱼中氯霉素残留量。方法样品采用乙酸乙酯为溶剂提取,无水硫酸钠脱水,提取液氮气吹干,以10%甲醇溶液溶解,冷冻除去脂肪,经C18固相萃取小柱净化,采用C18固相萃取柱分离,流动相甲醇-水,梯度洗脱,流速为1 m L/min,紫外检测波长280 nm。结果在0.1~5μg/m L范围内,氯霉素浓度和峰面积线性关系良好,精密度较好,相对标准偏差(relative standard deviation,RSD)在3.12%~7.53%之间,检测限为0.02μg/g,回收率80.5%~107.1%。结论该方法前处理方法简单、快捷,对实验员身体危害小,准确度较好,适用于罗非鱼中氯霉素含量的测定。

Objective To establish a method for determination of chloramphenicol residues in tilapia by high performance liquid chromatography. Methods The sample was extracted with ethyl acetate, dehydrated with anhydrous sodium sulfate, and the extraction liquid was blown by nitrogen. Then they were dissolved by 10% methanol solution, frozen to remove fat and purified by C18 solid phase extraction column. The sample was separated by C18 column with mobile phase of methanol and water at the rate of 1 m L/min and detected at the wavelength of 280 nm. Results In the range of 0.1-5 μg/m L, the linear relationship between the concentration of chloramphenicol and the peak area was good, and the precision was relatively good. The limit of detection was 0.02 μg/g. The recoveries were 80.5%-107.1% with relative standard deviations of 3.12%-7.53%. Conclusion This method is efficient, reliable and sensitive, which is suitable for determination of chlorampheniciol in tilapia.