Differential Pulse Voltammetric Determination of Clenbuterol with Fullerene Modified Electrode
摘 要
将1.08 mg富勒烯(C60)分散在10 mL二氯甲烷中,取40 μL悬浮液滴涂在玻碳电极表面,吹干后在1 mol·L-1氢氧化钾溶液中进行活化,制得C60修饰电极。用循环伏安法研究了修饰电极的电化学行为。结果表明:经氢氧化钾处理后的修饰电极,在5 mmol·L-1铁氰化钾溶液中,可见一对准可逆的氧化还原峰,且峰电流显著高于在裸玻碳电极和未处理电极上的峰电流。据此提出了用微分脉冲伏安法测定盐酸克伦特罗的方法。盐酸克伦特罗的浓度在0.1~20 μmol·L-1范围内与其氧化峰电流呈线性关系,检出限(3S/N)为3.26×10-2μmol·L-1。方法用于尿样分析,回收率在99.5%~110%之间。
Abstract
Fullerene (C60, 1.08 mg) was dispersed in CH2Cl2 (10 mL), and dropped on the surface of glassy carbon electrode (GCE), then activated in 1 mol·L-1 KOH solution to prepare C60 modified GCE (C60/GCE). Electrochemical behavior of the modified electrode was studied by cyclic voltammetry. As shown by the experimental results, a pair of quasi-reversible oxidation and reduction peaks was observed in 5 mmol·L-1 K3Fe(CN)3 solution at the modified electrode, and the peak currents were found to be higher than those obtained at bare GCE and unactivated modified electrode. Based on these findings, a selective method for determination of clenbuterol (CLB) by differential pulse voltammetry was proposed. Linear relationship between values of oxidation peak current and concentration of CLB was kept in the range of 0.1-20 μmol·L-1 with detection limit (3S/N) of 3.26×10-2μmol·L-1. The proposed method was used in the analysis of samples of urine, and values of recovery found were in the range of 99.5%-110%.
中图分类号 O657.1
所属栏目 工作简报
基金项目 国家自然科学基金项目(20977042)
收稿日期 2013/5/12
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备注刘艳丽(1986-),女,河南周口人,硕士研究生,主要从事电化学分析研究。
引用该论文: LIU Yan-li,ZHU Sheng-nan,Qi Yu-bing,SONG Qi-jun. Differential Pulse Voltammetric Determination of Clenbuterol with Fullerene Modified Electrode[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2013, 49(6): 669~672
刘艳丽,朱胜男,齐玉冰,宋启军. 富勒烯修饰电极微分脉冲伏安法测定盐酸克伦特罗[J]. 理化检验-化学分册, 2013, 49(6): 669~672
被引情况:
【1】张静,张静, "涂丝型聚氯乙烯膜-硫酸沙丁胺醇电极的研制与应用",理化检验-化学分册 50, 1220-1222(2014)
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参考文献
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【2】KESKIN S, OZER D, TEMIZER A. Gas chromatography-mass spectrometric analysis of clenbuterol from urine[J]. Journal of Pharmaceutical and Biomedical Analysis, 1998,18(4/5):639-644.
【3】CEBULJ K N, CESTNIK V. A case of enzyme immunoassay validation for the determination of clenbuterol residues in bovine urine[J]. International Journal of Environment and Pollution, 2007,31(1/2):135-141.
【4】邓光辉,陈盛余,高静,等.毛细管电泳电化学法分离检测盐酸克伦特罗、特布他林和沙丁胺醇[J].分析试验室, 2012,31(2):25-28.
【5】LIU Li-jing, PAN Hai-bo, DU Min, et al. Glassy carbon electrode modified with Nafion-Au colloids for clenbuterol electroanalysis[J]. Electrochimica Acta, 2010,55(24):7240-7245.
【6】梁荣宁,高奇,秦伟.分子印迹电位型传感器快速检测猪尿液中的克伦特罗[J].分析化学, 2012,40(3):354-358.
【7】KROTO H W, HEATH J R, O′ BRIEN S C, et al. C60: buckminsterfullerene[J]. Nature, 1985,318(6042):162-163.
【8】RAO C N R, SESHADRI R, GOVINDARAJ A, et al. Fullerenes, nanotubes, onions and related carbon structures[J]. Materials Science & Engineering, R: Reports, 1995,R15(6):209-262.
【9】GOYAL R N, GUPTA V K, CHATTERJEE S. Fullerene-C60-moddified edge plane pyrolytic graphite electrode for the determination of dexamethasone in pharmaceutical formulations and human biological fluids[J]. Biosensors and Bioelectronics, 2009,24(6):1649-1654.
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