铜/金修饰电极-阴离子交换色谱-直流安培法测定阿米卡星注射液组分

Determination of Amikacin in Pharmaceutical Injection Solutions by Anion Exchange Chromatography with Cu/Au Electrode for Amperometric Detection

建立了一种用阴离子交换色谱分离、以自制铜／金修饰电极为工作电极的直流安培电化学法（DC）直接检测硫酸阿米卡星注射液中主要组分及杂质含量的分析方法。考察了流动相浓度、测定电位等参数对色谱分离和测定的影响。在固定相为CarboPacPA10阴离子交换柱、流动相为26mmol／LNaOH的色谱条件下，检测电位为0．64V时，阿米卡星在0．0005-0．02g／L（r=0．9989）和0．02-0．2g／L（r=0．9991）两个浓度范围内呈线性。与裸Au电极在采用脉冲安培检测模式（PAD）时相比，电化学检测所需要的碱性强度低（pH〈13），而且测定灵敏度高，线性范围宽。本方法不需要柱前和柱后衍生化，能同时测定硫酸阿米卡星注射液中的主要组分和杂质组分。修饰电极制作方法简单，催化稳定性好，可望被应用到流动注射、毛细管电泳等其它流动体系中，对硫酸阿米卡星原料药、注射液等实际样品中的各组分进行测定。

A Cu/Au modified electrode was fabricated for DC amperometric detection of amikacin in pharmaceutical injection solutions by anion-exchange chromatography. Experimental conditions such as detection potential, concentration of mobile phase on chromatographic resolution and detection sensitivity were evaluated. The column was CarboPac PAl0, the mobile phase was 26 mmoL/L NaOH solution, the detection potential was 0.64 V, the standard curve of amikacin was rectilinear in the range of 0. 0005 - 0.02 g/L （ r = 0. 9989 ） and 0.02 - 0.2 g/L （ r = 0. 9991 ）. In contradistinction to bare Au electrode with PAD method, raising the pH of mobile phase for electrochemical detection to approximately 13 was not required, the catalytic sensitivity was higher and the linear range was wider. Without pre-and post-column derivatization, this method can simultaneously be used to determinate the main component and impurities in amikacin pharmaceutical injection solutions. Ease of preparation, being applied in DC detection mode and good catalytic stability confirmed the interests of this modified electrode as amperometric sensor applications in other flow-through systems.