摘要
基于在碱性介质中,甲磺酸帕珠沙星(PM)对钌联吡啶的电致化学发光信号有增敏作用,建立了检测PM的毛细管电泳-电致化学发光新方法。研究了检测电位、钌联吡啶浓度、磷酸盐缓冲液浓度和pH、进样高压、进样时间、运行高压等实验参数对PM检测的影响。在最佳实验条件下,检测电位1.15V;钌联吡啶浓度7mmol/L;检测池缓冲溶液36mmol/L(pH8.0);流动缓冲液20mmol/L(pH8.0);进样高压10kV;进样时间14s;运行高压15kV,在3min内可实现PM的分离检测,线性范围为0.02～10mg/L,相关系数r=0.9968,检出限(S/N=3)为4.0×10-3mg/L,对2.0mg/LPM进行测定,峰高和迁移时间的RSD分别为4.28%和1.89%(n=11)。本法具有简便、快速、灵敏、进样量少等特点,并且能有效避免干扰物质的影响,已成功用于实际样品(注射液、尿液)中PM含量的测定,并初步探讨了反应机理。
A novel and sensitive method has been established for the determination of pazufloxacin mesylas using capillary electrophoresis（CE） coupled with electrochemiluminescence（ECL） detection.It was based on the phenomenon that in base medium pazufloxacin mesylas enhanced the ECL intensity of tris（2,2＇-bipyridyl） ruthenium（Ⅱ）.The influence of several experiment factors such as the detection potential,the concentration of tris（2,2＇-bipyridyl） ruthenium（Ⅱ）,the concentration and the pH of phosphate buffer,the electrokinetic voltage,injection time and the separation voltage on the determination of pazufloxacin mesylas was explored.Under optimal conditions such as detection potential of 1.15 V,36 mmol/L of phosphate buffer（pH 8.0） containing 7 mmol/L tris（2,2＇-bipyridyl） ruthenium（Ⅱ） in CEL detection cell,running buffer of 20 mmol/L（pH 8.0）,sample injection of 14 s at 10 kV,separation voltage of 15 kV,the detection of pazufloxacin mesylas could be accomplishd within three minutes.The enhanced ECL intensity was linear with pazufloxacin mesylas concentration in the range of 0.02-10 mg/L（r=0.9968） with a detection limit（S/N=3） of 4.0×10^-3 mg/L.The relative standard deviations（RSD） of ECL intensity and the migration time for eleven continuous injections of 2.0 mg/L pazufloxacin mesylas were 4.8% and 1.9%,respectively.This method has the merits of simpleness,speediness,selectivity,little sample injection,and can successfully avoid the influencing of the interference.This method was successfully utilized to the assay of pazufloxacin mesylas in real samples including injection and human urine.An elementary mechanism was proposed to explain this phenomenon.
出处
《分析化学》
SCIE
CAS
CSCD
北大核心
2008年第7期941-946,共6页
Chinese Journal of Analytical Chemistry
基金
国家自然科学基金(No20472076)
河南省杰出人才创新基金(No421002300)资助项目
关键词
毛细管电泳
电致化学发光
钌联吡啶
甲磺酸帕珠沙星
Capillary electrophoresis,electrochemiluminescence,tris（2,2＇-bipyridyl） ruthenium（Ⅱ）,pazufloxacin mesylas
