液相色谱-串联质谱法同时测定养殖水体中孔雀石绿和结晶紫含量

Simultaneous determination of malachite green and crystal violet level in aquaculture water using HPLC-MS/MS

本研究建立了应用液相色谱-串联质谱(LC-MS/MS)同时测定养殖水体中孔雀石绿和结晶紫的含量的方法。水样经乙腈和二氯甲烷萃取浓缩,中性氧化铝小柱净化,1 m L 50%的乙腈-乙酸铵溶液定容,氘代孔雀石绿和氘代结晶紫内标法定量,液相色谱-三重四级杆串联质谱仪多反应监测扫描模式(MRM)检测养殖水体中孔雀石绿和结晶紫的含量。结果表明,方法的定量限为2.0 ng/L;标准曲线线性范围为0.2~20.0 ng/m L;加标水平在2.0~20.0 ng/L之间时,平均回收率为89.9%~102.0%,批内和批间相对标准偏差均小于10%。该方法稳定可靠,可适用于检测养殖水体中孔雀石绿和结晶紫的含量。

In this study,a high performance liquid chromatography-tandem mass spectrometric( HPLC-MS/MS)method has been adopted to determine stimultaneously malachite green and crystal violet in aquaculture water. Samples were extracted by acetonitrile and dichloromethane,neutral alumina column purification and constant volume with1 m L acetonitrile ammonium acetate solution prior to HPLC-MS/MS analysis. The analysis was carried out with the multi-reaction monitoring( MRM) mode and internal standard isotope dilution method was used for quantification.Calibration curves for malachite green and crystal violet exhibited good linearity over the concentration range from 0. 2 to 20. 0 ng/m L with quantification limits of 2. 0 ng/L. When the spiked level was 2. 0 to 20. 0 ng/L,average recovery rate was between 89. 9% and 102. 0%. Intraplate relative standard deviation was less than 10%,and inter-batch relative standard deviation was less than 10%. This indicated that the method was accurate and reliable to meet the requirements of detection for malachite green and crystal violet in aquaculture water. [Chinese Fishery Quality and Standards,2018,8( 1) : 49-54]