养殖水体中孔雀石绿高效液相荧光检测法的研究

Study on Determination of Malachite Green in Aquatic Water by HPLC with Fluorescence Detector

本研究探索了养殖水体中孔雀石绿的高效液相荧光检测方法,通过正交试验获得最佳抽提方案,并对硼氢化钾的还原效果及方法检测限进行了研究探讨。结果表明,抽提时间为5min,样品与二氯甲烷的比例为1:1,抽提两次的方案回收率最高;0.002g硼氢化钾即能将孔雀石绿完全还原而又不引起孔雀石绿的降解。本方法在0.5～800ng/ml范围内具有很好的线性,相关系数R为0.99977,最低检出限为0.2μg/L。采用不同的水质进行验证,回收率在86.8%～93.3%之间,相对标准偏差(RSD)为3.15%～8.12%。本方法提取快捷、简便,适用于大批量的抽样检测,可检测出水样中痕量的孔雀石绿,为水产养殖环境提供可行的监测手段,为水体中孔雀石绿的检测标准的制定提供依据。

HPLC with fluorescence detector method for the determination of malachite green （MG） and leucomalachite green in aquatic water was established. By orthogonal test the optimal extraction technology was establish. Reduction effect of KBH4 and limit of detection （LOD） of the method were studied. The optimal extraction conditions are extraction time 5 min, volume ratio of sample to dichloromethane 1：1 and extraction times two. MG can be completely reduced by 0.002 g KBH4. Good linear relationship ranges from 0.5 ng/ml to 800 ng/ml with correlation coefficient 0.99977. And the LOD is 0.2 μg/L. The recovery rates range from 86.8% to 93.3% with the relative standard deviations （RSD） of 3.15% to 8.12%. The method is suitable for the trace analysis of MG in aquatic water owing to its high efficiency and convenience.