CE-UV-Vis法测定鲫鱼中结晶紫

Determination of Crystal Violet in Carp by Capillary Electrophoresis with Ultraviolet Visible Detection

用毛细管电泳（CE）-紫外可见（UV-Vis）检测法测定鲫鱼中结晶紫残留量的新方法。样品中的结晶紫用硼氢化钾还原为其代谢产物隐色结晶紫;鲫鱼样品用乙腈提取,二氯甲烷萃取,浓缩净化后用毛细管电泳进样检测,外标法定量。结果表明：该方法能有效用于鲫鱼中结晶紫的分析检测。其最佳测定条件为：流动相,100 mmol/L磷酸-磷酸二氢钠缓冲溶液（pH4.0）;紫外检测波长267 nm;分离电压为12 kV。结晶紫标准工作液浓度范围为1~32μg/mL时线性关系良好,相关系数为0.9942。方法检出限和定量检出限均为2.9μg/kg。空白样品结晶紫添加水平为5、10、20μg/mL时平均回收率分别为83.97%、109.55%和88.45%,相对标准偏差分别为3.22%、5.05%和2.09%。

A new method was established to analysis crystal violet（CV） residues in carp.Crystal violet in samples was reduced to its metabolite leuco-crysial violet with potassium borohydride.The carp samples were firstly extracted with acetonitrile and dichhoromethane in sequence,then followed by concentration and purification,finally detected with capillary electrophoresis（CE） using external standard method for quantitative analysis.The results show that CE-UV-Vis could effectively analyse crystal violet in carp.The optimum conditions were as follow：mobile phase,100 mmol/L phosphate-sodium dihydrogen phosphate buffer solution（pH4.0）;UV detection wavelength,267 nm;separation voltage of 12 kV.The linear relationship was good when the crystal violet concentration range of standard working liquid was between 1 and 32 μg/mL,and the correlation coefficien was 0.9942.The detection threshold（CCα） and the detection capability（CCβ） were both 2.9 μg/kg.The precision of the method,expressed as RSD（n=6） values for the within-laboratory reproducibility,at the three add levels of LCV（5,10 and 20 μg/kg）,were 3.22%,5.05% and 2.09%,respectively,and the average recoveries were 83.97%,109.55% and 83.45%,respectively.