Abstract
In this study, a NiFe2O4-CQDs composite was synthesized and utilized to modify a glassy carbon electrode (GCE) for the simultaneous electrochemical detection of acetaminophen (ACP) and caffeine (CFE). The composite material was characterized using various techniques, including FTIR and PL spectroscopy, confirming its suitability for electrochemical applications. The DP-ASV method was employed to determine the limit of detection (LOD) for ACP and CFE, which were found to be 0.35 μM and 0.34 μM, respectively. The electrochemical method exhibited a wide linear range from 0.5 μM to 11.9 μM for both analytes. Optimized experimental conditions, including accumulation potential, accumulation time, and pulse amplitude, contributed to high sensitivity, reproducibility, and accuracy in detecting these compounds. Recovery studies in pharmaceutical samples demonstrated reliable results, with recoveries ranging from 94.2% to 103.2%. These findings suggest that the NIF-CQDs-modified GCE is a promising candidate for rapid and accurate electrochemical analysis of ACP and CFE in real-world applications.
References
- Habibi B, Jahanbakhshi M, Abazari M. A modified single-walled carbon nanotubes/carbon-ceramic electrode for simultaneous voltammetric determination of paracetamol and caffeine. Journal of the Iranian Chemical Society. 2014;11(2):511-21.
- Demir N, Atacan K, Ozmen M, Bas SZ. Design of a new electrochemical sensing system based on MoS2-TiO2/reduced graphene oxide nanocomposite for the detection of paracetamol. New J Chem. 2020;44:11759-67.
- Švorc Ľ, Strežová I, Kianičková K, Stanković DM, Otřísal P, Samphao A. An advanced approach for electrochemical sensing of ibuprofen in pharmaceuticals and human urine samples using a bare boron-doped diamond electrode. J Electroanal Chem. 2018;822:144-52.
- Kang X, Wang J, Wu H, Liu J, Aksay IA, Lin Y. A graphene-based electrochemical sensor for sensitive detection of paracetamol. Talanta. 2010;81(3):754-9.
- Palakollu VN, Chiwunze TE, Liu C, Karpoormath R. Electrochemical sensitive determination of acetaminophen in pharmaceutical formulations at iron oxide/graphene composite modified electrode. Arab J Chem. 2020;13:4350-7.
- Silva FWL, Name LL, Tiba DY, Braz BF, Santelli RE, Canevari TC, et al. High sensitivity, low-cost, and disposability: A novel screen-printed electrode developed for direct electrochemical detection of the antibiotic ceftriaxone. Talanta. 2024;266:125075.
- Kumar M, Bajpai Tripathy D, Madankar C, Pradhan S. Development and validation of Micellar Liquid Chromatography method for analysis of Paracetamol and Ibuprofen in tablets dosage form. J Indian Chem Soc. 2025;102:101887.
- Lentini G, Habtemariam S. Microchip capillary electrophoresis–electrospray ionization mass spectrometry analysis of paracetamol metabolites in human urine: An intriguing case. J Chromatogr A. 2014;1327:160.
- Lourenção BC, Medeiros RA, Rocha-Filho RC, Mazo LH, Fatibello-Filho O. Simultaneous voltammetric determination of paracetamol and caffeine in pharmaceutical formulations using a boron-doped diamond electrode. Talanta. 2009;78:748-52.
- Švorc L. Determination of caffeine: a comprehensive review on electrochemical methods. Int J Electrochem Sci. 2013;8:5755-73.
- Koblová P, Sklenářová H, Brabcová I, Solich P. Development and validation of a rapid HPLC method for the determination of ascorbic acid, phenylephrine, paracetamol and caffeine using a monolithic column. Anal Methods. 2012;4:1588.
- Torres AC, Barsan MM, Brett CMA. Simple electrochemical sensor for caffeine based on carbon and Nafion-modified carbon electrodes. Food Chem. 2014;149:215-20.
- Zeng Y-L, Huang Y-F, Jiang J-H, Zhang X-B, Tang C-R, Shen G-L, et al. Functionalization of multi-walled carbon nanotubes with poly (amidoamine) dendrimer for mediator-free glucose biosensor. Electrochem commun. 2007;9:185-90.
- Wu Y, Tang L, Huang L, Han Z, Wang J, Pan H. A low detection limit penicillin biosensor based on single graphene nanosheets preadsorbed with hematein/ionic liquids/penicillinase. Mater Sci Eng C. 2014;39:92-9.
- Tilahun Yai Feyisa, Shimeles Addisu Kitte DY, Gebretsadik1 and G. Simultaneous Electrochemical Determination of Paracetamol and Caffeine using Activated Glassy Carbon Electrode. Anal Bioanal Electrochem. 2020;12:93-106.
- Tu NTT, Sy PC, Thien TV, Toan TTT, Phong NH, Long HT, et al. Microwave-assisted synthesis and simultaneous electrochemical determination of dopamine and paracetamol using ZIF-67-modified electrode. J Mater Sci. 2019;54:11654-70.
- Fernandes DM, Silva N, Pereira C, Moura C, Magalhães JMCS, Bachiller-Baeza B, et al. MnFe2 O4@ CNT-N as novel electrochemical nanosensor for determination of caffeine, acetaminophen and ascorbic acid. Sensors Actuators B Chem. 2015;218:128-36.
- Latif IA, Merza SH. Fabrication of Functionalize Reduce Graphene Oxide and Its Application in Ampicillin Detection. Nanosci Nanotechnol. 2016;6:24-33.
- Tchoffo R, Ngassa GBP, Doungmo G, Kamdem AT, Tonlé IK, Ngameni E. Surface functionalization of natural hydroxyapatite by polymerization of β-cyclodextrin: Application as electrode material for the electrochemical detection of Pb (II). Environ Sci Pollut Res. 2022;29:222-35.
- BindiyaDey, Manoharan C, Bououdina M, Venkateshwarlu M, Murugan A. Enhanced magnetic, electrochemical and gas sensing properties of cobalt substituted nickel ferrite nanoparticles prepared by hydrothermal route. J Phys Chem Solids. 2023;178:111364.
- Narang SB, Pubby K. Nickel Spinel Ferrites: A review. J Magn Magn Mater. 2021;519:167163.
- Ding X, Niu Y, Zhang G, Xu Y, Li J. Electrochemistry in carbon‐based quantum dots. Chem Asian J. 2020;15:1214-24.
- Jihad KM, Roknabadi MR, Mohammadi M, Goharshadi EK. Reduced graphene oxide/TiO2/NiFe2O4 nanocomposite as a stable photocatalyst and strong antibacterial agent. Sustain Environ Res. 2023; 33.
- Holzinger M, Goff A Le, Cosnier S. Nanomaterials for biosensing applications: A review. Front Chem. 2014;2:1-10.
- Wang X, Feng Y, Dong P, Huang J. A Mini Review on Carbon Quantum Dots: Preparation, Properties, and Electrocatalytic Application. Front Chem. 2019;Volume 7 - 2019.
- Sheshmani S, Mardali M, Shokrollahzadeh S, Bide Y. Starch-derived carbon quantum dots: Unveiling structural insights and photocatalytic potential as a bio-sourced metal-free semiconductor. Int J Biol Macromol. 2024;271:132535.
- Sudaryanto Y, Hartono SB, Irawaty W, Hindarso H, Ismadji S. High surface area activated carbon prepared from cassava peel by chemical activation. Bioresour Technol. 2006;97:734-9.
- Tong S-K, Chi P-W, Kung S-H, Wei D-H. Tuning bandgap and surface wettability of NiFe2O4 driven by phase transition. Sci Rep. 2018;8:1338.
- Rao R, Zhang X, Sun X, Wang M, Ma Y. Effects of elemental chemical state in NiFe2O4@ TiO2 on the photocatalytic performance. J Wuhan Univ Technol Sci Ed. 2020;35:320-6.
- Bhosale S V, Kanhe NS, Bhoraskar S V, Bhat SK, Bulakhe RN, Shim J-J, et al. Micro-structural analysis of NiFe2O4 nanoparticles synthesized by thermal plasma route and its suitability for BSA adsorption. J Mater Sci Mater Med. 2015; 26:1–15.
- Fathy MA, Kamel AH, Hassan SSM. Novel magnetic nickel ferrite nanoparticles modified with poly(aniline- co-o -toluidine) for the removal of hazardous 2,4-dichlorophenol pollutant from aqueous solutions. RSC Adv. 2022;12:7433-45.
- Taqvi SIH, Solangi AR, Buledi JA, Khand NH, Junejo B, Memon AF, et al. Plant extract-based green fabrication of nickel ferrite (NiFe2O4) nanoparticles: An operative platform for non-enzymatic determination of pentachlorophenol. Chemosphere. 2022;294:133760.
- Stachowska JD, Gamża MB, Mellor C, Gibbons EN, Krysmann MJ, Kelarakis A, et al. Carbon Dots/Iron Oxide Nanoparticles with Tuneable Composition and Properties. Nanomaterials. 2022;12:1-18.
- Liu H, Liang J, Fu S, Li L, Cui J, Gao P, et al. N doped carbon quantum dots modified defect-rich g-C3N4 for enhanced photocatalytic combined pollutions degradation and hydrogen evolution. Colloids Surfaces A Physicochem Eng Asp. 2020;591:124552.
- Minh TT, Phong NH, Van Duc H, Khieu DQ. Microwave synthesis and voltammetric simultaneous determination of paracetamol and caffeine using an MOF-199-based electrode. J Mater Sci. 2018;53:2453-71.
- Katseli V, Economou A, Kokkinos C. A novel all-3D-printed cell-on-a-chip device as a useful electroanalytical tool: Application to the simultaneous voltammetric determination of caffeine and paracetamol. Talanta. 2020;208:120388.
- Monteiro MKS, Santos E, Silva DR, Martínez-Huitle CA, Dos Santos E V. Simultaneous determination of paracetamol and caffeine in pharmaceutical formulations and synthetic urine using cork-modified graphite electrodes. J Solid State Electrochem. 2020;24:1789-800.
- Phong NH, Toan TTT, Tinh MX, Tuyen TN, Mau TX, Khieu DQ. Simultaneous Voltammetric Determination of Ascorbic Acid, Paracetamol, and Caffeine Using Electrochemically Reduced Graphene-Oxide-Modified Electrode. J Nanomater. 2018;2018:1-15.

This work is licensed under a Creative Commons Attribution-ShareAlike 4.0 International License.
Copyright (c) 2025 Array