高效液相色谱法测定水产品中孔雀石绿及其代谢物的含量

Determination of Malachite Green and Its Metabolites in Aquatic Products by High Performance Liquid Chromatography

建立了高效液相色谱-荧光法测定水产品中孔雀石绿和隐色孔雀石绿的方法。样品经乙腈超声提取、硼氢化钾还原、离心、旋转蒸发及中性氧化铝柱净化后,经微孔滤膜过滤,滤液经液相色谱柱分离,荧光检测器检测,外标法定量。结果表明,孔雀石绿和隐色孔雀石绿在1.0~20.0μg·mL^(-1)均具有很好的线性关系,相关系数≥0.9998,检出限为0.5μg·kg^(-1),定量限为1.5μg·kg^(-1),加标回收率为88.1%~96.6%,RSD为0.9%~3.8%。

A method for the determination of malachite green and leucomalachite green in aquatic products by high performance liquid chromatography with fluorescence detection was established.After ultrasonic extraction with acetonitrile,reduction with potassium borohydride,centrifugation,rotary evaporation,purification with neutral aluminum oxide column,the sample is filtered by microporous membrane,and the filtrate is separated by liquid chromatography column,detected by fluorescence detector,and quantified by external standard method.The results showed that malachite green and leucomalachite green showed good linearity in the range of 1.0~20.0μg·mL^(-1) with the correlation coefficients≥0.9998,the limits of detection of 0.5μg·kg^(-1) and the limits of quantification of 1.5μg·kg^(-1),and the recoveries of spiked standards ranged from 88.1%to 96.6%with the RSD of 0.9%~3.8%.