高效阴离子交换色谱-铜/铂修饰电极安培法测定大观霉素  

Copper Modified Platinum Electrode for Amperometric Detection of Spectinomycin Sulfate by Anion Exchange Chromatography

作　　者：任丹丹[1] 习玲玲[1] 黄伟民[1] 朱岩[1] 

机构地区：[1]浙江大学西溪校区化学系,杭州310028

出　　处：《分析化学》2010年第11期1563-1567,共5页Chinese Journal of Analytical Chemistry

基　　金：国家自然科学基金(No.20775070);浙江省自然科学基金(No.4100190)资助

摘　　要：采用阴离子交换色谱分离,在CuSO4溶液中加入少量镧系化合物,经电沉积制备La3+-Cu/pt/CME工作电极,建立了直流安培电化学法(DC)直接检测硫酸大观霉素的方法。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CarboPac PA10阴离子交换柱、流动相为26mmol/L NaOH,流速为0.6mL/min的色谱条件下,检测电位为0.68V时,硫酸大观霉素峰面积与其浓度在0.12～12mg/L(r=0.9991)和12～280mg/L(r=0.9995)两个范围内呈线性。本方法不需要柱前和柱后衍生化,能同时测定硫酸大观霉素中的主要组分和杂质。修饰电极制作方法简单,催化稳定性好,可作为电化学传感器测定硫酸大观霉素中的各组分。A La3＋ -Cu/Pt modified electrode was fabricated by electrodepositing process in CuSO4 solution by adding a small amount of lanthium compound,and was employed for direct current （ DC） amperometric detection of spectinomycin 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 PA10,the mobile phase was 26 mmol/L NaOH solution,the flow rate of mobile phase was 0. 6 mL/min,the detection potential was 0. 68 V,the standard curve of spectinomycin was rectilinear in the range of 0. 12 12 mg/L （ r = 0. 9991） and 12 280 mg/L （ r = 0. 9995） . Without pre-and post-column derivatization,this method can be used to simultaneously determine the main component and impurities in spectinomycin pharmaceutical raw material. Ease of preparation,being applied in DC detection mode and good catalytic stability confirmed the interests of this modified electrode as amperometric sensor for the determination of spectinomycin.

关 键 词：铜/铂化学修饰电极 高效阴离子交换色谱 直流安培法 大观霉素 

分 类 号：S859[农业科学—临床兽医学]