液相色谱串联质谱法测定养殖水体中孔雀石绿及其代谢物

摘要

研究利用液相色谱-串联质谱(LC-ESI-MS/MS)测定水产品养殖水体中孔雀石绿及其代谢物隐性孔雀石绿的方法.通过一系列实验对样品前处理条件进行了优化研究,养殖水样经乙酸酸化,净化后,采用HPLC-ESI-MS/MS检测分析.在多反应监测模式(MRM)下,外标法定量,定量限均为0.5μg/kg.在0.5～50μg/L浓度范围内与峰面积线性关系良好(相关系数r>0.999),平均添加回收率71.5%～88.0%.该方法简便、高效、准确.适用于检测水样中痕量的孔雀石绿及其代谢物,为水产养殖环境提供可行的监测手段,同时可为水体中孔雀石绿检测标准的制定提供依据.%A new method for determination malachite green and its metabolites in aquatic water by ultra - performance liquid chromatography -electrospray ionization tandem mass spectrometry was developed.,Sample preparation and HPLC - MS/MS analytical conditions were examined and optimized critically by a series of experiments.Samples were acidulated by acetic acid , then cleaned up, and ultimately LC - ESI - MS/MS method was adopted for qualitative and quantitative analysis.Limit of detections (LOD) was 0.5 μg/kg.The method showed good linearity(r ＞0.999) at the rang of 0.5 -50 μg/L.The average recoveries ranged from 71.5％ to 88.0％.The method is suitable for the trace analysis of MG in aquatic water owing to its high efficiency and convenience, and it can provide a basis for testing standard of malachite green in water.