液相色谱-串联质谱法测定养殖水体中的孔雀石绿

Determination of malachite green level in aquaculture water by liquid chromatography-tandem mass spectrometry

应用液相色谱-串联质谱（LC-MS/MS）测定养殖水体中孔雀石绿的含量.水样经二氯甲烷萃取浓缩,以1 mL50％的乙腈-乙酸铵溶液定容,采用液相色谱-三重四级杆串联质谱仪多反应监测扫描模式（MRM）检测,使用氘代孔雀石绿内标法定量.检测方法的定量限为0.010 ng/mL,线性范围为0.25 ～ 10.0 ng/mL,加标浓度在0.005～0.100 ng/mL时,平均回收率在80％～110％,相对标准偏差小于10％.实验证明,该方法比较稳定,适用于检测养殖水体中孔雀石绿的含量.

In this study, a high performance liquid chromatography - tandem mass spectrometric （ HPLC - MS/MS） method has been adopted to determine malachite green in aquaculture water. Samples were subjected to extraction by dichloromethane, concentration and constant volume prior to HPLC - MS/MS analysis. The analysis was carried out in the multi -reaction monitoring （MRM） mode, and internal standard isotope dilution method was used for quantification. Calibration curves for malachite green exhibited good linearity over the concentration range from 0. 25 to 10.0 ng/mL, with quantification limits of 0.01 ng/mL, when the concentration degree was 0. 005 - 0. 100 ng/mL, the average recovery rate was 80% - 110%, and the relative standard deviation was less than 10%. It indicated that the method can meet the requirements of detection of malachite green in aquaculture water. [ Chinese Fishery Quality and Standards, 2015, 5（3）：34-39]