Instituto de Química de São Carlos, Universidade de São Paulo, C.P. 780, 13560-970, São Carlos, SP, Brazil.
Instituto de Química de São Carlos, Universidade de São Paulo, C.P. 780, 13560-970, São Carlos, SP, Brazil.
Talanta. 2020 Aug 1;215:120883. doi: 10.1016/j.talanta.2020.120883. Epub 2020 Mar 2.
This work describes the development, optimization, and validation of an electrochemical method for the determination of hydrochlorothiazide (HCTZ) in urine. The method allows fast, cheap and reliable determinations of recent administrations of this diuretic that can be used in doping control in sport. The response of the sensor was determined by differential pulse voltammetry (DPV). The glassy carbon electrode was modified with multiwall carbon nanotubes (MWCNT) and gold nanoparticles. The sensor is calibrated in the analysed sample matrix by the cumulative standard addition method. The method validation was based on the bottom-up evaluation of the measurement uncertainty were components were combined using the Monte Carlo Method (MCM) applicable with no restrictions regarding components uncertainty value and measurement function linearity. The developed metrological models were implemented in MS-Excel spreadsheets. The adequacy of the electrochemical measurements was assessed by comparing their relative standard uncertainty with a target value of 20% and by evaluating the compatibility of measurements with determinations performed by a reference procedure. The tools developed for the construction and optimization of working electrodes are applicable to measurements of other analytes and matrices. The used cumulative standard addition method and respective measurement uncertainty models are applicable to any kind of non-destructive chemical measurement of a solution.
本工作描述了一种用于测定尿液中氢氯噻嗪(HCTZ)的电化学方法的开发、优化和验证。该方法允许快速、廉价和可靠地测定这种利尿剂的最近给药情况,可用于运动中的兴奋剂控制。传感器的响应通过差分脉冲伏安法(DPV)确定。玻碳电极用多壁碳纳米管(MWCNT)和金纳米粒子修饰。通过累积标准加入法在分析样品基质中对传感器进行校准。方法验证基于测量不确定度的自下而上评估,其中使用蒙特卡罗法(MCM)组合各个分量,而不受分量不确定度值和测量函数线性度的限制。开发的计量模型在 MS-Excel 电子表格中实现。通过将相对标准不确定度与 20%的目标值进行比较,并通过评估测量与参考程序进行的测定的兼容性,评估电化学测量的充分性。用于构建和优化工作电极的工具适用于其他分析物和基质的测量。所使用的累积标准加入法和相应的测量不确定度模型适用于溶液的任何非破坏性化学测量。