毛细管电泳—电化学发光联用检测鱼露中苯乙胺

Determination and Separation of Phenylethylamine in Fish Sauce by Capillary Electrophoresis - Electrochemiluminescence Detection

基于苯乙胺与三联吡啶钌在铂电极表面上发生氧化反应,增强Ru(bpy)32+的ECL强度,将毛细管电泳-电化学发光联用应用于检测鱼露中苯乙胺的含量,分析影响苯乙胺发光强度的实验条件并进行优化。检测鱼露中苯乙胺含量的最优条件是:检测电位1.20V,光电倍增管高压800V,Ru(bpy)32+浓度5mmol/L(pH7.0),进样时间8s,进样高压12kV,运行缓冲液为pH7.0050mmol/L磷酸盐缓冲溶液。在优化条件下,1～40μg/mL质量浓度的苯乙胺与发光强度呈良好的线性关系,其线性方程为I=1.73c+9.71,相关系数r=0.9981,检出限(S/N=3)为0.06μg/mL。采用该方法测定鱼露中的苯乙胺,迁移时间和峰高的相对标准偏差(RSD)分别为0.08%和1.40%,加标回收率102.19%～108.08%。该方法的优点在于分析速度快,分离效果好,灵敏度高,重现性好。

CE/ Ru （bpy）3^2＋ electrochemiluminescence applied to the detection phenylethylamine content in fish sauce based on Phenylethylamine and tris（2,2＇-bipyridyl）ruthenium （II） [Ru （bpy）3^2＋] Oxidation on the surface of the platinum electrode enhance the ECL intensity of Ru （bpy）3^2＋. Experimental parameters influencing the effects of separation and luminous intensity were explored in details. Under the optimized conditions, such as detection potential at 1.20 V, photomuhiplier tube voltage at 800 V, 5 mmol/L Ru（bpy）3^2＋ （pH 7.0）, sample injection at 8 s×12 kV, separation voltage at 11 kV, 50 mmol/L of phosphate buffer at pH 7.0. Under the most qualified, the ECL intensity was linear with the concentration of phenylethylamine in the range of 1 -40μg/mL. The linear equation for I=1.73c ＋9.71, correlation coefficient r =0.9981 with detection limit （S/N=3） of 0.06 μmol/L. Determination of phenyl ethylamine in fish sauce, the relative standard deviation （RSD） of peak height and migration time were 0.08% and 1.40%. Recovery is 102.19%- 108.08%. This method is rapid analysis, good separation, high sensitivity and good reproducibility.