司帕沙星在单壁碳纳米管修饰电极上的电化学行为及其测定
Electrochemical Behavior of Sparfloxacin at SWCNT-film Modified Glassy Carbon Electrode and Its Application to the Determination of Sparfloxacin
摘 要
运用循环伏安法和线性扫描伏安法研究了司帕沙星在单壁碳纳米管修饰电极上的电化学行为,提出了一种简便、准确、灵敏的检测药物司帕沙星的电化学分析方法.在pH 6.0的0.1 mol·L-1 Na2HPO4-NaH2PO4缓冲溶液中,司帕沙星在单壁碳纳米管修饰电极上于1.06 V电位处有一峰形很好的氧化峰.在最佳的试验条件下,该氧化峰电流与司帕沙星的浓度分别在1.1×10-6~2.2×10-5mol·L-1和2.7×10-5~1.6×10-4mol·L-1范围内呈线性关系.在开路富集30 s的条件下测得方法的检出限(3S/N)为5.0×10-7mol·L-1.电极上的吸着物质经循环伏安扫描即可除去,从而使电极活性恢复,在SPFX浓度为4.0×10-5mol·L-1的浓度水平下用同一电极连续测定10次,求得相对标准偏差为5.1%,取片剂样品按提出方法分析,测定值与标示值相符.在此基础上用标准加入法作回收试验,测得回收率在97.6%~105.7%之间.
伏安测定
修饰电极
司帕沙星
Single-wall carbon nanotube
Voltammetry
Modified glassy carbon electrode
Sparfloxacin
Abstract
Electrochemical behavior of sparfloxacin (SPFX) at the single wall carbon nanotube (SWCNT) film modified glassy carbon electrode (GCE) was studied thoroughly by cyclic voltammetry and linear sweeping voltammetry.In a 0.1 mol·L-1 Na2HPO4-NaH2PO4 buffer solution of pH 6.0,a well-defined oxidation peak was observed at 1.06 V,and linear relationships between values of oxidation peak current and concentration of SPFX were obtained in 2 range sections,i.e.,from 1.1×10-6 to 2.2×10-5mol·L-1 and from 2.7×10-5 to 1.6×10-4mol·L-1.Detection limit (3S/N) of the method found under the condition of open-circuit accumulation for 30 s was 5.0×10-7mol·L-1.Adsorbed substances on the surface of the modified electrode were removed by cyclic voltammetric sweeping and thus making the electrode activity recovered.Ten determinations of SPFX with a same electrode at the concentration level of 4.0×10-5mol·L-1 were made to test for its precision,giving value of relative standard deviation of 5.1%.In analyzing a sample of SPFX tablet by the proposed method,the results obtained were in consistency with the labelled value.Test for recovery was made by the standard addition method based on the matrix of tablet sample,values of recovery found were in the range of 97.6%-105.7%.
中图分类号 O657.1
所属栏目 试验与研究
基金项目 国家自然科学基金(No.20775047)和河南省自然科学基金(No.0511022300)
收稿日期 2008/4/15
修改稿日期
网络出版日期
作者单位点击查看
备注徐茂田(1962-),男,河南夏邑人,教授,主要从事电化学分析研究.
引用该论文: XU Mao-tian,KONG Fen-ying,ZHANG Yin-tang. Electrochemical Behavior of Sparfloxacin at SWCNT-film Modified Glassy Carbon Electrode and Its Application to the Determination of Sparfloxacin[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(2): 134～137
徐茂田,孔粉英,张银堂. 司帕沙星在单壁碳纳米管修饰电极上的电化学行为及其测定[J]. 理化检验－化学分册, 2009, 45(2): 134～137
被引情况:
【1】徐茂田,朱效华, "单壁碳纳米管修饰电极循环伏安法测定盐酸利多卡因",理化检验－化学分册 49, 550-552(2013)
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【2】赫春香,赵常志,唐祯安.碳纳米管修饰电极对多巴胺和抗坏血酸的电催化氧化[J].分析化学,2003,31(8):958-960．
【3】Musamch M,Wang J,Merboci A.Low-potential stable NADH detection at carbon-nanotube-modified glassy carbon electrodes[J].Electrochem Commun,2002,4(10):743-746．
【4】曹书霞,张建业,姬小明,等.高效液相色谱法测定斯帕沙星注射液[J].色谱,2001,19(5):454-456．
【5】Marona H R N,Schapoval E E S.High-performance liquid chromatographic assay of sparfloxacin[J].J Pharm Biomed Anal,1999,20(3):413-417．
【6】杜黎明,卫洪清,郜艳,等.反相高效液相色谱法测定人尿中的司帕沙星[J].分析化学,2001,29(9):1108-1109．
【7】孙雨安,王国庆,崔泉中.司帕沙星含量的HPLC测定[J].分析测试学报,2000,19(1):62-64．
【8】Marona H R N,Schapoval E E S.Spectrophotometric determination of sparfloxacin in pharmaceutical formulations using bromothymol blue[J].J Pharm Biomed Anal,2001,26(3):501-504．
【9】陈晓芳,宣春生,李文英.司帕沙星与茜素红荷移反应的研究[J].分析试验室,2006,25(3):108-111．
【10】褚定侃,汪海波.紫外分光光度法测定司帕沙星注射液主含量[J].光谱实验室,2003,20(5):742-743．
【11】郑红莲,冯育林.痕量氟罗沙星和司帕沙星的荧光薄层色谱法测定[J].分析测试学报,2003,22(3):45-47．
【12】李华岑,高建华,龚雪云.曙红B荧光猝灭法测定司帕沙星[J].光谱实验室,2003,20(5):676-680．
【13】孙春燕,赵慧春,易琳,等.流动注射光化学敏化化学发光法测定斯帕沙星[J].分析化学,2002,30(8):920-924．
【14】石杰,曹丰璞,赵开楼,等.流动注射化学发光法测定司帕沙星的研究[J].分析试验室,2006,25(3):89-91．
【15】翟海云,谭学才,陈缵光,等.司帕沙星的毛细管电泳高频电导法测定[J].分析试验室,2004,23(11):26-29．
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【21】Rizk M,Belal F,Ibrahim F,et al.Voltammetric analysis of certain 4-quinolones in pharmaceuticals and biological fluids[J].J Pharm Biomed Anal,2000,24(2):211-218．
【22】Girish K K,Augustine P,Poduval R,et al.Voltammetric studies of sparfloxacin and application to its determination in pharmaceuticals[J].Pharmazie,2006,61(4):291-292．
【23】Cai Y,Zhang Y,Su S,et al.Electrochemical studies oxidation of ciprofloxacin at nano-SnO2/PVS modified electrode and its interaction with calf thymus DNA[J].Front Biosci,2007,12(1):1946-1955．
【24】Laviron E.General expression of the linear potential sweep voltammogram in the case of diffusionless electrochemical systems[J].J Electroanal Chem,1979,101:19-28．
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