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Journal Pre-proof Iron oxide (Fe2O3) nanoparticles modified carbon paste electrode as an advanced material for electrochemical investigation of paracetamol and dopamine M.M Vinay, Y Arthoba Nayaka PII: S2468-2179(19)30208-4 DOI: https://doi.org/10.1016/j.jsamd.2019.07.006 Reference: JSAMD 239 To appear in: Journal of Science: Advanced Materials and Devices Received Date: 10 April 2019 Revised Date: 22 July 2019 Accepted Date: 28 July 2019 Please cite this article as: M.M Vinay, Y Arthoba Nayaka, Iron oxide (Fe2O3) nanoparticles modified carbon paste electrode as an advanced material for electrochemical investigation of paracetamol and dopamine, Journal of Science: Advanced Materials and Devices, https://doi.org/10.1016/ j.jsamd.2019.07.006 This is a PDF file of an article that has undergone enhancements after acceptance, such as the addition of a cover page and metadata, and formatting for readability, but it is not yet the definitive version of record This version will undergo additional copyediting, typesetting and review before it is published in its final form, but we are providing this version to give early visibility of the article Please note that, during the production process, errors may be discovered which could affect the content, and all legal disclaimers that apply to the journal pertain © 2019 Publishing services by Elsevier B.V on behalf of Vietnam National University, Hanoi Iron oxide (Fe2O3) nanoparticles modified carbon paste electrode as an advanced material for electrochemical investigation of paracetamol and dopamine Vinay M Ma, Y Arthoba Nayakaa* a Department of Chemistry, School of Chemical Science, Kuvempu University, Shankaraghatta - 577451, Karnataka, India, tel.: +919448855078; fax: +9108282 256255 *Corresponding author E-mail address: drarthoba@yahoo.co.in (Y Arthoba Nayaka) Graphical abstract: CH3 O N NH Electrocatalysis O c b C urrent (µ Α ) O a - -20 a -80 b c Buffer BCPE -2e + -2H IOCPE NH CH -100 -120 -0.2 - -2e + -2H -40 -60 20 Dopamine-o-quinone Current (µ Α ) 20 O NAPQI 10 a b -10 -20 -30 a-Buffer c a-BCPE c-IOCPE -40 -50 0.0 0.2 0.4 0.6 Potential (V) vs Ag/AgCl 0.8 HN -0.1 O 0.0 0.1 0.2 0.3 0.4 Potential (V) vs Ag/AgCl IOCPE OH OH OH PA DA 0.5 To, Date 04.07.2019 The Editor, JSAMD Subject: Submission of Revised Manuscript With reference to the above subject, herewith I am submitting manuscript of the research paper your journal, which is entitled your journal, which is entitled “Iron oxide (Fe2O3) nanoparticles modified carbon paste electrode as an advanced material for electrochemical investigation of paracetamol and dopamine” The article is ORIGINAL and unpublished and is not being considered for publication elsewhere Kindly consider and the needful Thanking You, With Regards (Prof Y Arthoba Nayaka) Iron oxide (Fe2O3) nanoparticles modified carbon paste electrode as an advanced material for electrochemical investigation of paracetamol and dopamine Vinay M Ma, Y Arthoba Nayakaa* Abstract Electrochemical behaviors of paracetamol (PA) and dopamine (DA) have been investigated by cyclic voltammetry (CV), differential pulse voltammetry (DPV) and square wave voltammetry (SWV) using a selective and sensitive iron oxide (Fe2O3) nanoparticle modified carbon paste electrode (IOCPE) The PA and DA showed anodic peak potential at 0.458 V and 0.247 V and cathodic peak potential at 0.088 V and 0.11 V (vs Ag/AgCl), respectively In DPV mode PA and DA gave linear response over the concentration range of to 150 µM (R2 = 0.998) and to 170 µM (R2 = 0.989), respectively The limit of detection (LOD = 3s/m) for PA and DA were found to be 1.16 and 0.79 µM, respectively IOCPE possess excellent electrocatalytic activity towards the determination of PA and DA The proposed method could be successfully validated for the simultaneous and individual determination of PA and DA present in pharmaceutical and real samples Keywords: Carbon paste electrode; Differential pulse voltammetry; Electrochemical impedance spectroscopy; Iron oxide nanoparticles Graphical abstract: CH3 O N NH Electrocatalysis O c b C urrent (µ Α ) O a - -20 a -80 b c Buffer BCPE -2e + -2H IOCPE NH CH -100 -120 -0.2 - -2e + -2H -40 -60 20 Dopamine-o-quinone Current (µ Α ) 20 O NAPQI 10 a b -10 -20 -30 a-Buffer c a-BCPE c-IOCPE -40 -50 0.0 0.2 0.4 0.6 Potential (V) vs Ag/AgCl 0.8 HN -0.1 O 0.0 0.1 0.2 0.3 0.4 0.5 Potential (V) vs Ag/AgCl IOCPE OH OH OH PA DA Introduction Paracetamol (PA) (N-acetyl-p-aminophenol or acetaminophen) is one of the most widely used analgesic and antipyretic drug [1] PA release the pain associated with headache, backache, arthritis and postoperative effect, and it is commonly used for reducing the fever [2] PA having pKa value 9.5, rapidly gets distributed after oral administration and is easily excreted in urine PA does not exhibit any harmful side effects, but in few cases, it leads to the formation of liver damage and nephrotoxic metabolites [3] An overdose of PA leads to hepatic toxicity, liver and kidney damage and in some cases cause death [4] Dopamine (DA) another most leading catecholamine-based neurotransmitter drug and it was monitoring the central nervous system (CNS) and thus by arbitrating the multiple CNS functions such as memory, learning, neuroendocrine secretion, cognition and control of locomotion The difference in the concentration of DA level leads to severe causes such as Parkinson’s disease, depression, schizophrenia and Huntington’s disease, HIV infection, epilepsy and senile dementia [5] So, it is necessary to determine the drugs present in pharmaceutical samples and human biological fluids (urine and blood) Therefore, the development of simple, rapid, sensitive, and precise analytical procedures for the detection and quantification of these drugs is of great importance [6] Numerous methods are available for the determination of PA and DA such us spectrophotometry [7], TLC [8], HPLC [9-10], LC-MS [11], flow-injection analysis [12], UVVis spectrometry [13], electrochemical methods [14], fluorimetry methods [15] and chemiluminescence methods [16] The electrochemical techniques have received a remarkable consideration due to their unique qualities such as simple pretreatment procedure, good sensitivity, better selectivity, less time-consumption and low cost [17] In recent years, the modification of electrode surface fascinated significant attention because of their extremely enhanced sensitivities Literature survey reveals that PA and DA undergoes electrochemical reactions at different electrodes, such as graphite electrodes (GE) [18], polyurethane modified GE [19], glassy carbon electrodes (GCE) [20], modified GCE [21], screen-printed electrodes [22], carbon paste electrodes (CPE) [23], modified CPE [24], carbon fiber microelectrodes [25], carbon ionic liquid electrodes [26], platinum electrodes [27], gold electrodes [28] and boron doped diamond electrode (BDDE) [29] Currently, metal nanoparticles, nanodiamonds, fullerenes, carbon nanotubes, etc., were being used in biomedical and sensor applications, since nanomaterials possess fundamental features like smaller size, good optical, magnetic and mechanical properties [30] Metal nanoparticles have much more considerations during the last few decades due to their unique properties as well as a large surface-to-volume ratio as compared to their bulk counter parts [31] The various electrochemical methods are available for the determination of drugs and have been reported in the literature The modification of carbon paste electrode with different metal nanoparticles can improve the performance in terms of sensitivity and selectivity, and hence fastens the rate of electron transfer between the electroactive species and the electrode surface Several metal nanoparticles are reported in literature, such as platinum [32], gold [33], silver [34], copper [35] and as well as metal oxide nanoparticles MnO2 [36], NiO [37] CuO [38], and ZnO [39] these were used for the development of electrochemical sensors The Fe2O3 nanoparticles revealed sole features which powerfully differ from those of massiveness phases The electronic, magnetic and optical properties of Fe2O3 nanoparticles have a wide importance in many industrial applications including the extended new electronic, optical devices, information storage, magnetocaloric refrigeration, color imaging, bioprocessing, ferrofluid technology or the manufacture of magnetic recording media [40] The present work reports the determination of PA and DA simultaneously, using electrochemical techniques such as CV, DPV, SWV and EIS The analytical applications of IOCPE have been tested via the redox reaction of PA and DA present in biological (urine and serum) and pharmaceutical samples The proposed modified electrode IOCPE has got low limit of detection, good sensitivity, better selectivity and so it could be used for the estimation of PA and DA present in pharmaceutical and real samples Experimental 2.1 Apparatus All the voltammetric experiments were carried out using Electrochemical Workstation (Model number: CH Instrument 660D, USA) The electrochemical experiments were performed using conventional three-electrode system The IOCPE, platinum wire and silver/silver chloride were used as working, auxiliary and reference electrode, respectively The Equiptronics EQ-611 pH meter was used for the pH measurements All the electrochemical studies were carried under lab temperature 2.2 Chemicals and reagents The standard drugs Paracetamol (Acetaminophen) ( ≥ 99%) and Dopamine hydrochloride ( ≥ 99%) have been procured from Sigma Aldrich (USA and Germany, respectively), diPotassium hydrogen phosphate anhydrous ( ≥ 98%), Potassium hydrogen phosphate ( ≥ 98%) and Potassium chloride purified ( ≥ 99%) were procured from Merck (Mumbai, India) Silicon oil, Potassium ferricyanide (III) (99%, A.R.) obtained from Himedia (Mumbai, India) Paracetamol tablets and Dopamine injection tubes have been purchased from local market (Shivamogga, India) PBS of 0.1 M was prepared (lab temperature at 26±2 oC) and the pH was adjusted using NaOH and H3PO4 All the solutions were prepared using doubly distilled water 2.3 Procedure 2.3.1 Preparation of iron oxide nanoparticles (ION’s) Iron oxide nanoparticles have been synthesized by simple precipitation method under laboratory condition using FeCl3.6H2O and liquid ammonia The stoichiometric ratio of FeCl3.6H2O powder has been dissolved in doubly distilled water and stirred well To this constant stirring solution, 14 % of NH4OH solution has been added drop-wise (0.2 ml min-1) with maintaining the pH 8.0 The obtained brown coloured iron oxide was filtered The excess of base was washed with water and dried in an oven for about 12 h, and finally subjected to calcination at 500 oC for h The so obtained Fe2O3 sample has been characterized by scanning electron microscopy (SEM), energy dispersive X-Ray analysis (EDAX) and X-ray diffraction (XRD) techniques [41,42] 2.3.2 Preparation of bare carbon paste electrode (BCPE) and IOCPE The working electrode (IOCPE) was developed by mixing graphite powder, silicon oil and ION’s in the ratio 76:20:4 (w/w) and the resultant mixture were thoroughly homogenized using mortar and pestle The obtained paste was tightly packed into the glass tube (60 mm height, mm diameter) without any air gap The electrical contact has been made at one end by inserting a copper wire through the center of the paste packed glass tube without any crack The exposed end of the electrode was mechanically polished and renewed using butter sheet to get reproducible smooth and shiny working surface This operation has been repeated before start of each experiment The BCPE has been prepared in the same way without addition of modifier Result and Discussion 3.1 Characterization of prepared ION’s and IOCPE ... oxide (Fe2O3) nanoparticles modified carbon paste electrode as an advanced material for electrochemical investigation of paracetamol and dopamine? ?? The article is ORIGINAL and unpublished and is.. .Iron oxide (Fe2O3) nanoparticles modified carbon paste electrode as an advanced material for electrochemical investigation of paracetamol and dopamine Vinay M Ma, Y Arthoba... considered for publication elsewhere Kindly consider and the needful Thanking You, With Regards (Prof Y Arthoba Nayaka) Iron oxide (Fe2O3) nanoparticles modified carbon paste electrode as an advanced material