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吸附催化方波伏安法直接测定尿液中的二甲双胍。

Direct determination of metformin in urine by adsorptive catalytic square-wave voltammetry.

作者信息

Skrzypek Sławomira, Mirceski Valentin, Ciesielski Witold, Sokołowski Adam, Zakrzewski Robert

机构信息

Department of Instrumental Analysis, University of Łódź, Pomorska 163, 90-236 Łódź, Poland.

出版信息

J Pharm Biomed Anal. 2007 Oct 18;45(2):275-81. doi: 10.1016/j.jpba.2007.07.010. Epub 2007 Jul 12.

Abstract

A new adsorptive catalytic voltammetric method for voltammetric determination of metformin based on the catalytic hydrogen evolution reaction at a hanging mercury drop electrode was developed. The electrode reaction was analyzed under conditions of linear sweep voltammetry (LSV), differential pulse voltammetry (DPV) and Osteryoung-type square-wave voltammetry (SWV). The peak current depends on pH of the medium, concentration and chemical composition of the buffer solution, and instrumental parameters. The optimal conditions for quantitative determination were obtained in an acetate buffer at pH 4.7. The voltammetric procedure was characterized with respect to the repeatability, precision and the recovery. The detection and quantification limits were found to be 1.8 x 10(-8) and 5.9 x 10(-8) mol l(-1) for SWV, 3.2 x 10(-8) and 1.0 x 10(-7) mol l(-1) for DPV, and 7.7 x 10(-8) and 2.5 x 10(-7) mol l(-1) for LSV, respectively. The SW voltammetric method, as the most sensitive one, was applied for determination of metformin in human urine. The voltammetric method has been validated by using HPLC with UV detection.

摘要

基于悬汞滴电极上的催化析氢反应,开发了一种用于伏安法测定二甲双胍的新型吸附催化伏安法。在线性扫描伏安法(LSV)、差分脉冲伏安法(DPV)和奥斯特杨型方波伏安法(SWV)条件下对电极反应进行了分析。峰电流取决于介质的pH值、缓冲溶液的浓度和化学成分以及仪器参数。在pH 4.7的乙酸盐缓冲液中获得了定量测定的最佳条件。对伏安法的重复性、精密度和回收率进行了表征。SWV的检测限和定量限分别为1.8×10⁻⁸和5.9×10⁻⁸ mol·L⁻¹,DPV为3.2×10⁻⁸和1.0×10⁻⁷ mol·L⁻¹,LSV为7.7×10⁻⁸和2.5×10⁻⁷ mol·L⁻¹。作为最灵敏的方法,SW伏安法用于测定人尿中的二甲双胍。伏安法已通过使用带紫外检测的高效液相色谱法进行了验证。

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