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建立了运动员营养补剂中3种人体必需支链氨基酸(缬氨酸、亮氨酸、异亮氨酸)的毛细管电泳-电容耦合非接触电导检测(CE-C4D)测定方法。通过研究电泳时背景电解质种类、浓度以及电导检测器的激发电压,激发频率等参数的影响,确定最佳的实验条件为采用未涂层熔融石英毛细管(60 cm×75μm,有效长度50 cm),以5.0 mol/L的乙酸为背景电解质;C4D检测器激发电压为40 V,激发频率为600 kHz;运行电压为+15 kV,温度为25℃。3种氨基酸在50.0~1000.0μmol/L范围内线性关系良好,线性相关系数(R2)均大于0.9994,加标回收率在98.6%~105.4%之间,方法的检出限为14.88μmol/L。方法已应用于运动员蛋白营养补剂中的支链氨基酸的测定。
A capillary electrophoresis-capacitively-coupled noncontact detection (CE-C4D) method for determination of three kinds of essential branched chain amino acids (valine, leucine and isoleucine) in human nutrition supplements was established. The optimum experimental conditions were determined by using uncoated fused silica capillary (60 cm × 75 μm, effective length 50 cm) by studying the influence of the type and concentration of background electrolyte and the excitation voltage and excitation frequency of the conductivity detector. With 5.0 mol / L acetic acid as the background electrolyte, the excitation voltage of C4D detector was 40 V and the excitation frequency was 600 kHz. The operating voltage was +15 kV and the temperature was 25 ℃. The linearity of the three amino acids in the range of 50.0 ~ 1000.0μmol / L was good, and the linear correlation coefficients (R2) were all above 0.9994. The recoveries of the three amino acids ranged from 98.6% to 105.4%. The detection limit was 14.88μmol / L. The method has been applied to the determination of branched-chain amino acids in athlete nutritional supplements.