采用毛细管电泳-电化学检测法(CE-ED),对饲料中的6种磺胺类药物磺胺脒、磺胺二甲嘧啶、磺胺甲嘧啶、磺胺二甲氧嘧啶、磺胺嘧啶、磺胺甲恶唑进行了分离和测定。分别考察了工作电极电位、运行缓冲液的pH和浓度、分离电压和进样时间等实验参数对实验结果的影响。在优化的实验条件下,以直径300μm的碳圆盘电极为工作电极,检测电位为0.95 V(vs.SCE),在30 mmol/L硼砂-KH2PO4(pH7.6)的运行缓冲溶液中,6个分析物能够在16 min内实现很好的基线分离,被测物浓度与峰电流在3个数量级呈良好的线性,检出限(S/N=3)范围0.08~0.20μg/mL。该方法已应用于实际样品的分析。
A method based on capillary electrophoresis with electrochemical detection(CEED) has been developed for the separation and determination of six sulfonamides (sulfaguanidine,sulfamethazine,sulfamerazine,sulfadimethoxine,sulfadiazine,and sulfamethoxazole) in feed.The effects of working electrode potential,pH and concentration of running buffer,separation voltage,and injection time on CE-ED were investigated.Under the optimum conditions,the six analytes could be separated within 16 min at a separation voltage of 18 kV in 0.30 mol/L borate -0.40 mol/L phosphate running buffer(pH 7.6).A 300 μm diameter carbon disk electrode generated good responses at 0.95 V(vs.SCE) for the six analytes.The response was linear over three orders of magnitude with detection limits(S/N=3) ranging from 0.08 to 0.20 μg/mL for the analytes.This proposed method was successfully applied to the analysis of the practical samples,with satisfactory assay results.