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methods and objects of chemical analysis 2021 vol 16 no 2 103 111 voltammetric determination of paracetamol in pharmaceutical formulations at iodine coated polycrystalline platinum electrode mohammad amayreh wafa hourani ...

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             Methods and objects of chemical analysis, 2021, Vol. 16, No. 2, 103–111
             Voltammetric Determination of Paracetamol in Pharmaceutical 
             Formulations at Iodine-Coated Polycrystalline Platinum Electrode 
                                       †                 ‡                                §
             Mohammad Amayreh* , Wafa Hourani , Mohammed Khair Hourani
             † Department of Chemistry, Faculty of Science, Al-Balqa Applied University, P.O. Box 19117, Al-Salt, Jordan; *e-mail: 
             mohammad.amayreh@bau.edu.jo
             ‡ Faculty of Pharmacy, Philadelphia University, Amman, Jordan
             § Department of Chemistry, the University of Jordan, Amman, Jordan
             Recieved: April 05, 2021;  Accepted: May 31, 2021
             DOI: 10.17721/moca.2021.103-111
             Copyright © 2021 Amayreh Mohammad et al. Open access article distributed under the Creative Commons 
             Attribution License CC BY 4.0.
                      In this work the modified iodine-coated polycrystalline platinum electrode was used to develope a voltammetric 
                      sensor for paracetamol determination in pharmaceutical formulations. The optimized experimental parameters for 
                      the determination of paracetamol were using 0.5 M H SO  as a supporting electrolyte with a scan rate of 50 mV/s. 
                                                                           2    4
                      The anodic peak related to paracetamol oxidation was centered at about +0.60 V. The extended calibration graph 
                                                                                                                         2
                      was constructed between 1 ppm and 500 ppm. The anodic current showed excellent linearity with R  = 0.9985. The 
                      limit of detection (LOD) and limit of quantitation (LOQ) were 0.046 and 0.139 ppm, respectively, which attests to 
                      the sensitivity of the method. The investigation for the effect of potential interferences from the content of tablet 
                      matrices indicated a specific selectivity toward paracetamol and the absence of any electrochemical response 
                      toward these components. The developed method was successfully applied to analysis paracetamol  in three 
                      brands of pharmaceutical formulations and the obtained results were in good agreement with the labeled values, 
                      besides that, the statistical tests indicated no significant difference at p = 0.05 with a 95 % confidence level.
                      Keywords: paracetamol, pharmaceutical formulation, voltammetric analysis, iodine-coated platinum electrode, 
                      modified platinum electrode
                   Determination of paracetamol in pharmaceutical            surface. Where the adsorbed iodine monolayer at 
             formulations is of great importance. Paracetamol                platinum electrode surface transforms the highly 
             (acetaminophen) is one of the most common drugs                 reactive surface to an apparent passive electrode with 
             around the world used for relief fever, headaches,              a low current background [25].
             and minor pain [1]. Also, paracetamol is renowned                   Iodine is one the anions simply adsorbed to 
             as multimodal analgesia with excellent safety profile           electrode surface. The chemisorptions process  can  be 
             except in significant overdoes [2] .Since paracetamol           achieved by two ways; from solution or from vacuum to 
             found solely or in combination in pharmaceutical                form stable chemisorbed mono layers even the iodine 
             formulation, it is a paramount important to have a              coated electrode would be rinsed or evacuated [26]. 
             simple, fast, sensitive, and selective analytical method        The iodine is adsorbed at potential 0.2 V (double layer 
             for routine analysis of this compound.                          potential) vs. Ag/AgCl or SCE reference electrodes 
                 A numerous analytical methods have been                     [27]. At the surface of polycrystalline platinum 
             reported for paracetamol determination in pharma-               electrode an oxidation reaction of iodine anions 
             ceutical formulations. These methods include,  from solution leads to spontaneous chemisorption of 
             potentiometry [3-7], high performance liquid  iodine anion to form stable neutral iodine atoms at 
             chromatography [8-13], and spectrophotometry [14] .             the electrode surface accompanied by hydrogen gas 
             These reported methods have some limitations such               evolution. The adsorbed iodine is less reactive toward 
             as instruments, skills, cost, and the environment.              electrochemical oxidation compared with the free 
             In contrast to these traditional methods, the  iodine anion in solution [28]. The chemisorbed iodine 
             electrochemical methods have attracted much  can be desorbed from platinum electrode surface if 
             attention due to the low sensitivity toward the matrix          the potential scanned lower than - 0.2 V which lead to 
             effects  compared  to  other  analytical  techniques            reduction of hydrogen ions and generation hydrogen 
             [15]. Also, the electroanalytical methods offer many            gas [28]. Also the rate of iodine desorption from 
             advantages such as simple analysis procedures,                  electrode surface increase as the potential become 
             environmentally–friendly chemical reagents. Many                more negative [29]. At the positive direction, the 
             voltammetric methods based on modified electrodes               chemisorbed iodine begins to be desorbed at potential 
             have been reported for paracetamol determination                1.0 [27]. Carbon monoxide is completely desorbed 
             in pharmaceutical tablets [16-24]. The Iodine-coated            iodine from platinum electrode surface at potential 
             platinum electrode considers as a typical example for           lower than 0.35 V while at higher potential incomplete 
             the modification of a highly reactive platinum electrode        desorption is occurred [30].
             Mohammad Amayreh, Wafa Hourani, Mohammed Khair Hourani                                                                 103
               Voltammetric determination of paracetamol in pharmaceutical formulations at iodine-coated polycrystalline platinum electrode
                Iodine-coated platinum electrodes have been            in 0.5 M H SO + 10-2 M KI solution  for  five  minutes 
                                                                                   2   4 
            applied  for  the  electrochemical  quantification  of     under closed-circuit potentiostatic conditions in the 
            some species in aqueous solutions with and without         double layer region  (~ 0.2 V)  to accomplish dosing  
            further  modification.  A  furtherly  modified  iodine-    of the platinum electrode surface with iodine. After 
            coated platinum electrode with quanternized poly(4-        that the electrode was subjected to multiple rinses 
            vinylpyridine), qPVP by Cox and Kulesa  was used for       with water and 0.5 M H SO  solution, and then 
                                                                                                  2   4
            analysis of nitrite [31]. Amayreh and co-workers have      the electrode potential was cycled in supporting 
            used the iodine-coated electrode for the analysis of       electrolyte solution between -0.2 V and +0.8 V at 
            iron(II) [32, 33] and copper(II) [34].                     50 mv/s to confirm the completeness of the coating 
                 Iodine-coated platinum electrode is characterized     process (Fig.1). The absence of oxygen and hydrogen 
            by the simplicity in preparation, application, and         adsorption/desorption peaks from the recorded 
            the absence of the need for environmentally  cyclic voltammogram of an iodine-coated platinum 
            unfriendly chemical reagents.  The simplicity of the       electrode provides a conclusive evidence for the 
            instrumentations all stimulated the implementation         complete coverage of platinum electrode surface with 
            of the present work. This work was undertaken with         a monolayer of   iodine.
            the  main objective of method development  for                 Standard  solution  preparation.  A 1000 ppm of  
            voltammetric analysis of paracetamol at iodine-coated      paracetamol stock solution  was prepared by dissolving  
            platinum electrode  in pharmaceutical formulations.        a 0.1g of paracetamol (151.163 g/mol) in 100mL of  
                                                                       0.5 M  H SO . A working solution of different concen-
            Experimental part                                                  2   4
                                                                       trations of paracetamol, 1, 10, 50, 100, 200, 300, 400, 
                Chemicals and reagents. The following reagents         and 500 ppm in 0.5 M H SO  were prepared through a 
                                                                                               2    4
            along with their suppliers were used in the present        serial dilution procedure.
            work: Sulfuric acid (95-97 %, Merck), paracetamol              Sample     preparation. The pharmaceutical 
            (99.8 %, Merck), potassium iodide (Sigma-Aldrich).         formulation samples (Paracetamol commercial 
            Milli-Q water (Millipore) was used for preparation of      tablets), Revanin (Jordan), Panda (Jordan), 
            all  solutions. The nitrogen gas was a five-G grade,       and   Myogesic (Jordan) were purchased from 
            99.999 % minimum purity supplied from International        Jordanian local drug stores. The selected brands of 
            Jordanian  Gases  Company  (Amman,  Jordan).  All          pharmaceutical formulations were analyzed for their 
            used chemicals and reagents were of analytical grade       paracetamol content. The tablet of each brand was 
            and used without further purification.                     powdered using porcelain mortar and dissolved in 
                Apparatus. A potentiostat (PAR Model 362,              warm 50.0 mL of 0.1 M H SO  supporting electrolyte 
                                                                                                  2   4
            EG & G) interfaced to a computer via GPIB interface        to ensure complete dissolution of paracetamol. 
            (IEEE)  equipped  with  a  locally  modified  Labview®     The solution of the samples was sonicated for  
            (IEEE) software was used for data acquisition and          5 minutes and left to equilibrate for 10 minutes. Then, 
            experimental control. A one-compartment electro-           the solution was filtrated through a 0.45 µm Millipore 
            chemical cell with an inlet/outlet system for deo-         filter and transferred to 100 mL volumetric flask and 
            xygenation and blanketing with highly pure nitrogen        diluted to the mark. The stock solutions were kept in 
            was used. A 0.5 mm polycrystalline platinum wire           the refrigerator for succeeding analysis. An aliquot 
            purchased from Aldrich (99.99 % minimum purity             of this solution was diluted to 50.00 mL with 0.1 M 
            certified reagent) was used as a working electrode. The    HSO to be within the constructed calibration curve 
                                                                         2   4
            immersed end of the platinum electrode was curved          concentrations’ range. A 10.00 mL of the diluted 
            at the end to make a mark for a consistent surface         solution was placed in the electrochemical cell. The 
            area of the immersed part of the electrode. A silver/      solution was deaerated with nitrogen gas and kept 
            silver chloride wire was used as a quasi-reference         under a nitrogen gas atmosphere during conducting the 
            electrode (QRE). The used auxiliary electrode was a        voltammetric measurements. Voltammetric analysis of 
            0.5 mm polycrystalline platinum wire (Aldrich, certified   the commercial tablets for their paracetamol content 
            99.99 % minimum purity).                                   was conducted  at the iodine-coated electrode within 
                Preparation  of  iodine-coated  platinum  electrode.   a potential window -0.2 V to  0.8 V where the adsorbed 
            Preparation of iodine-coated platinum electrode was        iodine is stable within this potential range. 
            described in one of our earlier publications [32], These   Results and discussions
            preparation steps include a cyclization of a platinum 
            electrode placed in of 0.5 M H SO  between - 0.25V and         Electrochemical  oxidation  of  paracetamol  and 
                                         2   4
            1.3 V until getting a reproducible   cyclic voltammogram   method validation
            of polycrystalline platinum electrode with the well-           Initially, as presented in Figure 1-a, a reproducible 
            known oxygen and hydrogen adsorption/desorption            cyclic voltammogram for polycrystalline platinum 
            features, which is indicative of the cleanliness of the    electrode was obtained which confirms the cleanness 
            electrode surface and electrochemical cell contents        of all components of the electrochemical system. On 
            (Fig.1).                                                   the other hand, the cyclic voltammogram of the iodine-
                Thereafter, the clean electrode was immersed           coated electrode (Fig.1-b) indicates a complete and 
             104                                           Methods and objects of chemical analysis, 2021, Vol. 16, No. 2, 103–111
                                           Mohammad Amayreh, Wafa Hourani, Mohammed Khair Hourani
             successful as witnessed by absence of any surface                    150
             activity in the scanned potential range (- 0.2 – 0.80  V). 
             The complete absence of hydrogen and oxygen                          100
             reduction features is the main evidence for complete                A 50
             coverage of the platinum surface. The potential scan                µ
                                                                                 /
             was limited to the above-mentioned range to avoid                   t  0
                                                                                 n
             desorption of iodine from the platinum surface. The                 rre
             adsorbed iodine is stable toward rinsing with acidic or             Cu-50
             neutral supporting electrolytes. Also, the iodine-coated            -100
             platinum electrode does not need to regenerate before                         0.1 M KCl   0.1 M H2SO4   Phosphate Buffer, pH=3.5
             each measurement  where scanned potential window                    -150
             should between -0.2 and 1.0 V, which indicates to                       -0.2      0       0.2      0.4      0.6      0.8
             reliability of using the electrode for daily routine                                  Potential/V vs. Ag/AgCl
             analysis.
                                                                                       140
                   800                                                                 120    117.7±1.73
                   600                                                                                    100.31±1.83
                                                                                       100                              87.82±3.56
                 A 400                                                               µA
                 µ                                       A                           /  80
                 nt/200                                                              ent
                 e                                                                   r  60
                 r   0                                                               ur
                 ur                         B                                        C  40
                 C -200
                                                                                        20
                   -400
                   -600                                                                  0
                                                                                             0.5M H2SO4    Phosphate     0.1M KCl
                   -800                                                                                      buffer
                       -1      -0.5      0       0.5       1        1.5       Fig. 2.  Effect of type of supporting electrolyte on the 
                                  Potential /V vs. Ag/AgCl                    electrochemical signal of paracetamol at iodine-
             Fig. 1. Cyclic voltammogram curves of (a) poly-                  coated platinum electrode, Paracetamol; 100 ppm, 
             crystalline platinum electrode and(b) the same                   HSO; 0.5 M, phosphate buffer; pH=3.5; KCl, 0.1 M; 
                                                                -2              2   4
             electrode after adsorption of iodine from 1x10  MKI in           n = 3; scan rate, 50 mV/sec.
             0.5 M H SO  solution.
                      2    4                                                      The effect of scan rate from 10 mV/s to 100 mV/s 
                 The effect of pH on the iodine coating on platinum           on the paracetamol peak current was evaluated. As 
             electrode has been reported elsewhere [35] where it              presented in Figure 3, there is a linear relationship 
             has been found that iodine coating is unstable upon              between the square root of scan rate and the oxidation 
             cyclization in basic solution [36] . This fact limits usage      peak current of paracetamol: y = 14.798 x - 10.932; 
                                                                                 2 
             of iodine-coated electrode to acidic solutions only.  The        (R = 0.9976), which indicates that the oxidation 
             effect of the pH in the acidic range was investigated by         process is a diffusion-controlled process. 
             following the effect of pH change on the peak current                  200
             for paracetamol oxidation. Three representative pH                                    ―10mv/sec
             values; 7, 3.5 and 0.3 were selected to demonstrate                    150            ―20 mv/sec
             the effect of solution acidity on the analytical signal 
             (peak current). Paracetamol standard solution was                   A  100            ―50 mv/sec
             analyzed in 0.5 M H SO   (pH = 0.3),  phosphate                     µ
                                                                                 /
                                        2    4                                   t
             buffer  (pH = 3.5),  and  0.1M  KCl  (pH = 7)  media.               n   50
             Figure 2 shows the effect of pH on the paracetamol                  rre
             oxidation current peak.  As displayed in Figure 2, the              Cu   0
             value of the oxidation peak current of paracetamol                     -50
             decreases with increasing pH. Thereafter, 0.5 M 
             HSO was considered as a supporting electrolyte                        -100
               2    4 
             for determination of paracetamol the following                        -150
             study. This might be attributed to the experimentally                     -0.2      0        0.2      0.4       0.6      0.8
             evidenced observation that the protonated form of                                   Potential /V vs. Ag/AgCl
             the paracetamol is more easily oxidized than the 
                                         
             deprotonated form [37].The ease of oxidation of the              Fig. 3. Cyclic voltammograms of iodine-coated 
             protonated form of paracetamol is revealed by the                platinum electrode in 0.5M H SO  containing 50 ppm 
                                                                                                               2   4
             shift in paracetamol peak potential with increasing pH           of paracetamol at various scan rates: 10, 20, 50, and 
             of the medium.                                                   100 mv/s. 
             Methods and objects of chemical analysis, 2021, Vol. 16, No. 2, 103–111                                                  105
                Voltammetric determination of paracetamol in pharmaceutical formulations at iodine-coated polycrystalline platinum electrode
                 The obtained cyclic voltammograms for iodine-                     700
             coated platinum electrode in a series of paracetamol                        Y = 1.1517X+1.0592
                                                                                          2 
             standard solutions show that the oxidation current                    600   R = 0.9985                          572 ± 10
             increases linearly with paracetamol concentration. 
             Three voltammograms were recorded for each                            500
             standard solution and the dimensions of each point                   A                                     465 ± 2
             were displayed in Figure 4. The anodic peak current                  µ400
                                                                                  /
             was extracted for each cyclic voltammogram.                          nt                            355 ± 2 
                                                                                  e
                                                                                  r
                                                                                  ur300
                    600                                                           C
                                    ―50 ppm                                        200                  212 ± 3
                    500             ―100 ppm
                                                                                   100           113 ± 2
                    400             ―200 ppm                                                  56 ± 2
                 A                  —300 ppm                                                12 ± 1
                 µ  300                                                             0     6 ± 1
                 /                  ―400ppm                                           0      100     200     300     400     500     600
                 nt
                 e  200                                                                               Concentration (ppm)
                 r
                 Cur100                                                       Fig. 5. An extended calibration curve shows the 
                      0                                                       relationship between paracetamol concentration 
                                                                              in ppm and the oxidation peak current measured 
                    -100                                                      from cyclic voltammograms for paracetamol in  
                                                                              0.5 M  H SO  at iodine-coated platinum electrode. 
                    -200                                                                2   4      -1
                       -0.2      0       0.2      0.4      0.6      0.8       Scan rate = 50  mv.s .
                                   Potential /V vs.Ag/AgCl                        Where paracetomol is a phenolic compound that 
             Fig. 4. Cyclic voltammograms of iodine-coated  undergoes electrochemical oxidation by electrolytic 
             platinum electrode in 0.1 M H SO  solution containing            etching on the aromatic ring with irreversible removal 
                                              2   4                           of two electrons and two protons, producing N-ace-
             50, 100, 200, 300 and 400 ppm of paracetamol. All the            tyl-p-quinoneimine according to the mechanism 
             scans were recorded at a scan rate of 50 mV/s.
                                                                              shown in equation [37] :
                  Figure 5 shows a representative part of the cyclic 
             voltammograms  recorded for a standard solutions                      O             OH                   O
             of paracetomol used for construction calibration                                                                           +2e-   +2H+
             curve. The established calibration curve between                                                    H C     N + 2e- + 2H+
                                                                              HC      N                            3
             concentrations  of 50, 100, 200, 300 and 400  ppm                  3     H
             and the current values extracted from the recorded 
             cyclic voltammograms shows a linear relationship with 
                                     2 
             regression value of R = 0.986.                                                                              O
                 Plotting the anodic peak current variation against 
             paracetamol concentration give a straight and                        The inter-and intra-day precision was estimated 
             extended dynamic range with a concentration ranging              by  extracting  the  current  values  for  four  different  
             from 1.0 ppm to 500.0 ppm. The calibration curve                 paracetamol standard solutions sample between 10 
             displayed in Figure 5 shows remarkable linearity; 
               2                                                              and 200 ppm. The standard deviation was found to be 
             R = 0.9985, and the calibration equation is given by             within 0.49 and 2.79 for five successive determinations 
                 I = (µA) = 1.1517 Cparacetamol+ 1.0592                       for each concentration. The measured values of 
                 where I represents the anodic peak current, which            standard deviation attest to the high repeatability for 
             attributed to the paracetamol oxidation.                         both of inter-and intra-day measurements.
                                                                                  The limit of detection based on the formula 
                 The 95 % confidence intervals (α = 0.05, 6 degrees           LOD = 3.3Ϭ/S, and limit of quantitation based on the 
             of freedom) for the slope  and y-intercept are                   formula LOQ = 10Ϭ/S, where Ϭ represents the blank 
             β1=b ± ts = 1.15 ± 2.5 x 0.0232 = 1.152 ± 0.057                  signal (background current) and S represents the 
                   1    b1                                                    sensitivity of the calibration curve was calculated 
             β2=b ± ts = 1.059 ± 2.5 x 5.90 = 1.0 ± 14                        [38]. The estimated limits were 0.046 ppm and 0.139 
                   0    b0 
                                                                              ppm respectively. Acceptable sensitivity of the applied 
                                                                              method with high precision was obtained. A higher 
                                                                              sensitivity can be achieved by application of a more 
                                                                              sensitive technique like differential pulse voltammetry. 
                                                                              Differential  pulse  voltammetry,  however,  was  not 
              106                                                Methods and objects of chemical analysis, 2021, Vol. 16, No. 2, 103–111
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...Methods and objects of chemical analysis vol no voltammetric determination paracetamol in pharmaceutical formulations at iodine coated polycrystalline platinum electrode mohammad amayreh wafa hourani mohammed khair department chemistry faculty science al balqa applied university p o box salt jordan e mail bau edu jo pharmacy philadelphia amman the recieved april accepted may doi moca copyright et open access article distributed under creative commons attribution license cc by this work modified was used to develope a sensor for optimized experimental parameters were using m h so as supporting electrolyte with scan rate mv s anodic peak related oxidation centered about v extended calibration graph constructed between ppm current showed excellent linearity r limit detection lod quantitation loq respectively which attests sensitivity method investigation effect potential interferences from content tablet matrices indicated specific selectivity toward absence any electrochemical response t...

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