{"title":"Electrochemical detection of hydrochlorothiazide in the prescence of amlodipine and valsartan using FeMOF/g-C3N5−Modified Carbon Paste Electrode","authors":"Ziaie Neda, Sayed Mehdi Ghoreishi","doi":"10.1016/j.electacta.2025.146665","DOIUrl":null,"url":null,"abstract":"<div><div>A novel electrochemical sensor based on a carbon paste electrode (CPE) modified with nitrogen-doped graphitic carbon nitride and an iron-based metal-organic framework (FeMOF/g-C<sub>3</sub>N<sub>5</sub>) was developed for the sensitive detection of hydrochlorothiazide (HCTZ). The synthesized FeMOF/g-C₃N₅ nanocomposite was characterized using Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS), which confirmed its successful synthesis and structural integrity. Electrochemical characterization through cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) demonstrated significantly enhanced electron transfer properties, reducing the charge transfer resistance from 8865 Ω (bare CPE) to 517 Ω and increasing the peak current from 9.59 μA cm⁻<sup>2</sup> to 61.17 μA cm⁻<sup>2</sup>. Under optimized conditions (PBS 0.1 M, pH 7.0, scan rate of 0.1 V/s, 250 mV modulation amplitude, 25 mV step potential), the sensor showed a linear response to HCTZ over two ranges: 0.005–0.7 µM and 5.00–100.0 µM, with a detection limit of 1.30 nM and a sensitivity of 41.475 μA/μM. Chronoamperometric analysis indicated an irreversible diffusion-controlled process with a diffusion coefficient of 2.4 × 10⁻<sup>5</sup> cm<sup>2</sup>/s. The sensor exhibited excellent selectivity, enabling the simultaneous determination of HCTZ, amlodipine, and valsartan, with well-separated signals. Recovery studies in pharmaceutical tablets, human plasma, and urine samples yielded values between 93.33 % and 110 %, confirming the accuracy of the method for complex matrices. The synergistic integration of FeMOF and g-C<sub>3</sub>N<sub>5</sub> provides a high-performance sensing interface, offering a cost-effective and sensitive approach for the electrochemical detection of HCTZ in clinical and pharmaceutical applications.</div></div>","PeriodicalId":305,"journal":{"name":"Electrochimica Acta","volume":"536 ","pages":"Article 146665"},"PeriodicalIF":5.5000,"publicationDate":"2025-06-06","publicationTypes":"Journal Article","fieldsOfStudy":null,"isOpenAccess":false,"openAccessPdf":"","citationCount":"0","resultStr":null,"platform":"Semanticscholar","paperid":null,"PeriodicalName":"Electrochimica Acta","FirstCategoryId":"88","ListUrlMain":"https://www.sciencedirect.com/science/article/pii/S0013468625010266","RegionNum":3,"RegionCategory":"材料科学","ArticlePicture":[],"TitleCN":null,"AbstractTextCN":null,"PMCID":null,"EPubDate":"","PubModel":"","JCR":"Q1","JCRName":"ELECTROCHEMISTRY","Score":null,"Total":0}
引用次数: 0
Abstract
A novel electrochemical sensor based on a carbon paste electrode (CPE) modified with nitrogen-doped graphitic carbon nitride and an iron-based metal-organic framework (FeMOF/g-C3N5) was developed for the sensitive detection of hydrochlorothiazide (HCTZ). The synthesized FeMOF/g-C₃N₅ nanocomposite was characterized using Fourier-transform infrared spectroscopy (FT-IR), X-ray diffraction (XRD), scanning electron microscopy (SEM), and energy-dispersive X-ray spectroscopy (EDS), which confirmed its successful synthesis and structural integrity. Electrochemical characterization through cyclic voltammetry (CV) and electrochemical impedance spectroscopy (EIS) demonstrated significantly enhanced electron transfer properties, reducing the charge transfer resistance from 8865 Ω (bare CPE) to 517 Ω and increasing the peak current from 9.59 μA cm⁻2 to 61.17 μA cm⁻2. Under optimized conditions (PBS 0.1 M, pH 7.0, scan rate of 0.1 V/s, 250 mV modulation amplitude, 25 mV step potential), the sensor showed a linear response to HCTZ over two ranges: 0.005–0.7 µM and 5.00–100.0 µM, with a detection limit of 1.30 nM and a sensitivity of 41.475 μA/μM. Chronoamperometric analysis indicated an irreversible diffusion-controlled process with a diffusion coefficient of 2.4 × 10⁻5 cm2/s. The sensor exhibited excellent selectivity, enabling the simultaneous determination of HCTZ, amlodipine, and valsartan, with well-separated signals. Recovery studies in pharmaceutical tablets, human plasma, and urine samples yielded values between 93.33 % and 110 %, confirming the accuracy of the method for complex matrices. The synergistic integration of FeMOF and g-C3N5 provides a high-performance sensing interface, offering a cost-effective and sensitive approach for the electrochemical detection of HCTZ in clinical and pharmaceutical applications.
期刊介绍:
Electrochimica Acta is an international journal. It is intended for the publication of both original work and reviews in the field of electrochemistry. Electrochemistry should be interpreted to mean any of the research fields covered by the Divisions of the International Society of Electrochemistry listed below, as well as emerging scientific domains covered by ISE New Topics Committee.