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为建立1种快速检测水产品中组氨酸含量的方法,采用毛细管电泳(CE)分离-三联吡啶钌[Ru(bpy)32+]电化学发光(ECL)检测联用,研究电位、进样量、毛细管电泳高压、缓冲液pH等条件对信号强度、迁移时间的影响。结果显示,检测的最佳条件是:检测电位1.05 V,Ru(bpy)32+浓度5mmol/L(溶于pH8.0的磷酸盐缓冲溶液),进样时间12 s,进样高压10 kV,运行高压14 kV;运行缓冲溶液pH 8.0。在此条件下对组氨酸标准品进行快速检测,得到其线性方程为I=0.9082c-48.72,相关系数r=0.9985(n=5),检出限(S/N=3)为0.668μmol/L。采用该方法测定金线鱼样品中的组氨酸,得到峰高和迁移时间的相对标准偏差(RSD)值分别为0.25%和0.06%,加标回收率为92.81%和104.39%。该方法可应用于金线鱼中组氨酸含量的测定,具有高效、高灵敏度、样品消耗少及操作成本低的优点,为此方法应用于其他水产品中氨基酸的检测提供了试验基础。
In order to establish a rapid method for the determination of histidine in aquatic products, capillary electrophoresis (CE) separation - Ru (bpy) 32+] electrochemiluminescence (ECL) Volume, high pressure capillary electrophoresis, buffer pH and other conditions on signal intensity, migration time. The results showed that the optimal conditions for the detection were as follows: the detection potential was 1.05 V, the concentration of Ru (bpy) 32 + was 5 mmol / L (dissolved in phosphate buffer solution of pH 8.0), the injection time was 12 s, Operating high voltage 14 kV; running buffer pH 8.0. Under these conditions, the standard test of histidine was carried out. The linear equation was I = 0.9082c-48.72, the correlation coefficient was 0.9985 (n = 5), the detection limit (S / N = 3) was 0.668μmol / L. Using this method, the relative standard deviations (RSDs) of peak height and migration time were 0.25% and 0.06%, respectively, and the recoveries were 92.81% and 104.39%, respectively. The method can be applied to the determination of histidine in golden fish, which has the advantages of high efficiency, high sensitivity, less sample consumption and low operation cost, and provides experimental basis for the application of the method to the detection of amino acids in other aquatic products.