Materials Sciences and Applicatio n, 2011, 2, 957-963
doi:10.4236/msa.2011.28128 Published Online August 2011 (http://www.SciRP.org/journal/msa)
957
A Study on Preparation and Use of Nano Poly
Pyrrole and Nano Poly
(3,4-Ethylenedioxythiophene) Coated Glassy
Carbon Electrode for the Determination of
Antihistamine in Pharmaceutical and Urine
Sample
Balathandapani Muralidharan1*, Gopalakrishnan Gopu2, Saraswathy Laya1, Chinnapiyan Vedhi3,
Paramasivam Manisankar2
1Department of Chemistry, Birla Institute of Technology and Science-Pilani, Dubai Campus, Dubai, U.A.E; 2Department of Indus-
trial Chemistry, Alagappa University, Tamilnadu, India; 3Department of Chemistry, V.O. Chidambaram College, Tamilnadu, India.
Received September 25th, 2010; revised December 30th, 2010; accepted May 17th, 2011.
ABSTRACT
Pheniramine maleate (PA), an antihistamine, was determined by Differential Pulse Stripping voltammetry using nano
polypyrrole (Ppy) and nano po ly (3,4-ethylenedioxythiophene) (PEDOT) modified glassy carbon electrodes. The cyclic
voltammetric behavior of pheniramine was studied in aqueous acidic, neutral and alkaline cond itions. One well-defined
oxidation peak was ob served in the cyclic voltammograms at a ll pHs. The influence of pH , scan rate and concentration
revealed irreversible electron transfer and the oxidation was diffusion controlled adsorption. The SEM analysis con-
firmed good accumulation of PA on the electrode surface. A systematic study of influence of various experimental pa-
rameters that affect the stripping voltammetric response was carried out and the maximum peak current conditions
were arrived at. Calibration was made under maximum peak current conditions. The range of study was 0.05 to 0.4
 g/mL on Ppy/GCE and 0.025 to 0.4  g/mL on PEDOT/GCE and the lower limit of determination were 0.035  g/mL on
Ppy/GCE and 0.016
 g/mL on PEDOT/GCE. The suitability of the method for the determination of PA in pharmaceu-
tical preparations and urine samples was also ascertained.
Keywords: Pheniramine ma leate, Cyclic voltammetry, Stripping voltammetry, Nano polypyrrole, Nano poly
(3,4-ethylenedioxythiophene)
1. Introduction
Pheniramine maleate (PA), an antihistamine used to treat
allergic conditions such as hay fever or urticaria, has
relatively strong sedative effects. Because of this, the
determination of PA becomes important. High-perfor-
mance liquid chromatographic method for the quantita-
tive determination of PA in plasma has been developed
and validated by El-Sayed et al. [1]. Stability tests
showed that PA was stable for at least 3 weeks in plasma
after freezing. The chromatographic determination of
antihistaminic drugs, loratadine and PA from human se-
rum was also developed [2]. Thin-layer chromatography
densitometry was used to separate, identify and quant ate
chlorpheniramine maleate and PA when present in com-
bination with other drugs in pharmaceutical preparations
of tablets, syrups, eye and ear drops, etc. [3]. A new
chemiluminescence method, using flow injection, was
described for the determination of diphenhydramine hy-
drochloride and chlorpheniramine maleate [4].
Several high performance liquid chromatographic
procedures have been developed for the determination of
chloropheniramine maleate in commercial pharmaceuti-
cal preparations [5-7] and derivative spectrophotometry

A Study on Preparation and Use of Nano Poly Pyrrole and Nano Poly(3,4-Ethylenedioxythiophene) Coated Glassy Carbon 958
Electrode for the Determination of Antihistamine in Pharmaceutical and Urine Sample
[7-9]. A micellar electrokinetic chromatographic method
has also been described for simultaneous determination
of paracetamol and chlorpheniramine maleate [10]. High-
pressure liquid chromatograph using an intermediate
polarity column was reported for the determination of
four antihistamines such as brompheniramine maleate,
chlorpheniramine maleate, PA and pyrilamine maleate in
combination has been discussed. The potentiation of
apomorphine-induced gnawing by antihistamines might
depend upon the reciprocal balance between dopaminer-
gic and cholinergic systems. High-pressure liquid chro-
matographic determination of methscopolamine nitrate,
phenylpropanolamine hydrochloride, pyrilamine maleate,
and pheniramine maleate in tablets was also developed.
Enantioselective determination of PA in pharmaceuticals
by capillary electrophoresis with charged cyclodextrin
was studied by Peter Mikus et al. [11]. Analysis of enan-
tiomers in biological matrices by charged cyclodextrin-
mediated capillary zone electrophoresis in column-arrange-
ment with capillary sotachophoresis has been discussed
[12]. Cyclodextrin-mediated capillary isotachophoresis in
cationic regime of the separation has also been developed
for the separation and quantitation of alkylamine antihis-
tamine dimethindene and pheniramine enantiomers in
various pharmaceutical preparations [13]. Simultaneous
determination of pseudoephdrine, pheniramine, guaifen-
isin, pyrilamine, chlorpheniramine and dextromethorphan
in cough and cold medicines by high performance liquid
chromatography has been reported [14]. Recently aceta-
minophen, caffeine and chlorpheniramine maleate in tab-
let formulations has been simultaneously determined by
simple HPLC method [15].
In the past decades, conducting polymer modified
electrodes have received great attention due to their ex-
cellent characteristics, including high stability and selec-
tivity, good reproducibility and conductivity, more active
sites and good homogeneity [16-18]. They are widely
applied in many areas, such as molecule or ion recogni-
tion [16], electrocatalysis [19], electron transfer [20]. The
modified electrode was characterized by electrochemical
method [21] and the method proposed was successfully
applied to the determination of phenylephrine and chlor-
prothixene in drug injections or tablets and proved to be
reliable compared with ultraviolet spectrophotometry.
The application of conjugated polymers as sensor has
been exploited as active sensing elements by coupling
ligands to the backbone. Here, the binding of an analyte
results in physical distortion or changes in electron den-
sity, there by altering conductivity [22].
Nanomaterials of conjugated polymers are found to
have superior performance relative to conventional mate-
rials due to their much larger exposed surface area [23].
Shamsipur et al. has been studied nano-structured con-
ducting polymer and its application to the design of reli-
able scaffolds for impedimetric biosensors [24]. Ad-
vancement of in the design of innovative microbicide
nanocarriers and nano-enabled microbicides has also
been discussed [25].
Electrochemical methods have proved to be highly
sensitive for the analysis of drugs in pharmaceutical
formulations and human body fluids owing to the sim-
plicity, low cost and relatively short analysis time as
compared to the other routine analytical techniques in-
cluding chromatography. Perusal of literature reveals that
there are no publications concerning the electroanalytical
determination of pheniramine maleate in pharmaceutical
formulations. Therefore, the aim of the present investiga-
tion is to investigate the voltammetric behavior of phen-
iramine maleate in an attempt to develop a simple and
reliable electrochemical method for its determination in
pharmaceutical formulations and human urine.
2. Experimental
2.1. Apparatus and Reagents
EG&G M 273A Electrochemical Analyzer—Princenton
Applied Research Corporation (PARC) was employed
mainly for carrying out electroanalytical studies. The
pheniramine (PA) was purchased from SIGMA and used.
The stock solution was made up in double distilled
TKA-LAB purified water. For the electrochemical stud-
ies, Britton Robinson buffers, 0.1 mol·dm–3 KOH, KCl
and H2SO4 were used as the medium for the analysis. 3,
4-Ethylenedioxythiophene (Bayer), Pyrrole (AR-Merck)
and tetra butyl ammonium perchlorate (Sigma) were used
for electropolymerisation.
2.2. Procedure
Purging of nitrogen was done for analyte solution placed
in the electrochemical cell of 15 ml capacity for 20 min-
utes under stirred conditions. Various voltammograms
were recorded while nitrogen gas was blanketed. To get
reproducible results, great care was taken in the electrode
pretreatment. The glassy carbon electrode was pretreated
in two ways: mechanical polishing over a velvet mi-
cro-cloth with an alumina suspension and electrochemi-
cal treatment by applying a potential of 1.5 V for 2 sec-
onds.
2.3. Preparation of Nano Polypyrrole Coated
Glassy Carbon Electrode (Ppy/GCE)
Polypyrrole films were deposited on GCE by the elec-
trooxidation of 0.1 M pyrrole in acetonitrile containing
0.1 M tetrabutyl ammonium perchlorate at 0.0 to 0.90 V

A Study on Preparation and Use of Nano Poly Pyrrole and Nano Poly(3,4-Ethylenedioxythiophene) Coated Glassy Carbon 959
Electrode for the Determination of Antihistamine in Pharmaceutical and Urine Sample
(vs. Ag/AgCl) applied potential [26,27]. Thickness of the
films was controlled by number of cycles and 0.1 thick
films were used in all cases.
2.4. Preparation of Nano Poly
(3,4-ethylenedioxythiophene) Coated Glassy
Carbon Electrode (PEDOT/GCE)
Poly (3,4-ethylenedioxythiophene) films were deposited
on GCE by the electrooxidation of 0.01 M 3,4-ethylene-
dioxythiophene in acetonitrile containing 0.1M tetrabutyl
ammonium perchlorate (TBAP). The polymerisation of
this monomer was carried out voltammetrically by giving
multi cycle in the potential range between –0.2 and 1.2 V
at 50 mV/s using Ag/AgCl reference electrode [28].
Thickness of the film was controlled colulometrically
and 0.1 thick films were used in all cases. The SEM
photograph reveals the deposition of nano size (100 nm)
PEDOT on GCE.
Care was taken to remove the coating and clean the
glassy carbon electrode after every experiment in 1:1
HCl/water and 1:1 H2O2/acetic acid mixture before usual
surface treatment. Nitric acid (6 M) solution was used to
clean the cell.
The electrode stability of polypyrrole, PEDOT modi-
fied electrode is of prime importance in these studies.
The electrode was prepared quickly and found to be sta-
ble in the medium. It showed slight decrease in peak
current after 15 days of its preparation and thus it is
recommended that it should not be used after 15 days
because the peak current values start decreasing. The
response time of the electrode was very fast and all
measurements were carried out easily and quickly.
3. Results and Discussions
3.1. Effect of pH
Effect of pH was studied in detail by choosing thirteen
different pH conditions between 1.0 to 13.0. The pH of
the supporting electrolyte has a significant influence on
the electrooxidation of pheniramine at the modified elec-
trodes. The peak potential and the current were measured
by recording cyclic voltammograms at different pHs at a
sweep rate, 100 mV/s on nano Ppy/GCE and PE-
DOT/GCE. The peak potentials showed decreasing trend
with pH (Figure 1) while the peak current showed in-
creasing trend with pH (Figure 2). Since the protonated
substrate is oxidised at basic media, the maximum peak
current was observed only at pH 13.0. Because of the
low energy requirement and high electron transfer rate at
pH 13.0, it was considered as the most suitable pH for
the electroanalytical studies of pheniramine.
0
20
40
60
80
100
120
140
160
180
0 2 4 6 8101214
pH
ip(A)
Ppy
PEDOT
Figure 1. Plot of peak current vs. pH on two different elec-
trodes.
0
200
400
600
800
1000
1200
0 2 4 6 8101214
pH
E(mV)
Ppy
PEDOT
Figure 2. Plot of peak potential vs. pH on two different
electrodes.
3.2. Electrochemical Studies of Drug on
Modified Electrode
A representative cyclic voltammogram is presented in
Figure 3 on polymer modified GCE. The plot of peak
current vs scan rate (showed linear relationship. A
straight line with better correlation coefficient was ob-
tained when plotting ip vs square root of suggesting dif-
fusion-controlled adsorption of PA on both electrodes.
Another correlation of log peak current with log scan rate
resulted in straight line and slope value obtained is
0.4817 for Ppy and 0.4833 for PEDOT. These values are
closer to 0.5 confirming diffusion controlled adsorption.
There was no counter peak in the reverse scan and n
value was fractional. Increase in the concentration of PA
showed increased peak current and gradual increase in
peak potential. The plot of ip vs. C was also linear. All
these studies reveal that the electron transfer taking place
in the redox process is irreversible and the oxidation is
diffusion-controlled adsorption. Among the two modified
systems, the PEDOT/GCE was selected as a better elec-
trode system for the electroanalytical determination of
PA due to higher peak current.
3.3. Rate Constant
The standard rate constant ks was calculated from the

A Study on Preparation and Use of Nano Poly Pyrrole and Nano Poly(3,4-Ethylenedioxythiophene) Coated Glassy Carbon
Electrode for the Determination of Antihistamine in Pharmaceutical and Urine Sample
960
-25
25
75
125
175
-1000 -50005001000
E(mV)
i(A)
PEDOT
Ppy
Figure 3. Cyclic voltammogram of 250 mg/mL PA on dif-
ferent electrode at pH 13.0; scan rate 100 mV/s.
slope of log ip vs E – Ei plot by employing the following
equation.
ip = nFACks exp [–  n/RT(E – Ei)]
where ip = peak current in A, n = number of electrons
transferred, F = Faraday constant, 96487 C, A = area of
the electrode in cm2, C = concentration of the analyte,
mole s / c m3, ks = standard rate constant, cm/s,
 = transfer
coefficient, R = gas constant (8.314), T = temperature in
K, E = peak potential in V, Ei = potential at the foot of
the response in V.
The ks value for the electrooxidation of PA was 6.451
× 10–6 cm/s on Ppy/GCE and 3.76 × 110–5 cm/s on PE-
DOT/GCE. The lower value of rate constant ks confirms
that electron transfer is irreversible.
3.4. Differential Pulse Stripping Analysis of
Drugs (DPSV)
Adsorptive stripping voltammetry involves two steps in
which the first step is accumulation of the substrate on
the electrode and the second step involves stripping.
Cyclic voltammetric results revealed the good accumula-
tion of the substrate on electrode at pH 13.0 and hence
adsorptive stripping voltammetric studies performed well
in the determination of drug.
The pH, accumulation potential and time were varied
independently at default experimental conditions and
maximum peak current parameters were found out. The
solution was stirred throughout the accumulation period.
The accumulation of the drug on the modified electrode
surface under the optimum accumulation conditions
was confirmed from the changes in the electrode sur-
face before and after accumulation. SEM was employed
to study the surface morphology of the accumulated PA
on nano coated glassy carbon electrodes. Figure 4(a)
and 4(b) shows the small uniform granular nano Ppy
and irregular granular nano PEDOT surface. The drug
PA adsorbed on nano Ppy electrode during accumula-
tion and exhibited sponge like structure (Figure 4(c))
and nano PEDOT exhibited broken leaves structure
(Figure 4(d)).
The stripping parameters were varied and optimized.
The range of study and optimized values are presented in
Table 1. Under optimum experimental conditions, the
influence of concentration on the stripping signal was
studied. The experimental results showed that the peak
current increased with the increase in the concentration
of PA. A representative differential stripping voltammo-
gram is presented in Figure 5. Calibration was made and
the straight line plot is presented in Figure 6. The lower
limit of detection (LOD) determined from the peak cur-
rent obtained using nano Ppy is 0.035 g/mL and it is
0.016 g/mL using nano PEDOT (Table 2). The repro-
ducibility of the stripping signal was understood from the
relative standard derivation (2.8%) calculated for five
identical measurements at a concentration level of 0.2
g/mL. The LOD values obtained from this study for the
Figure 4. SEM photographs of (a) Nano Ppy (b) Nano PE-
DOT (c) PA on Nano Ppy and (d) PA on Nano PEDOT.
10
30
090
E(mV)
i(A)
0
10
35
0 900
E(mV)
i(A)
(a) (b)
Figure 5. DPSV behaviour of 0.2 g/mL PA on (a) Ppy and
(b) PEDOT.

A Study on Preparation and Use of Nano Poly Pyrrole and Nano Poly(3,4-Ethylenedioxythiophene) Coated Glassy Carbon 961
Electrode for the Determination of Antihistamine in Pharmaceutical and Urine Sample
Table 1. Optimum parameters condition of stripping voltammetry of pheniramine on modified glassy carbon electrode.
Ppy PEDOT
Parameters Range examined Optimized value Range examined Optimized value
pH 1.0 to 13.0 13.0 1.0 to 13.0 13.0
Accumulation potential (mV) 450 to 650 500 350 to550 500
Deposit time (sec) 10 to 60 10 10 to 60 10
Initial scan potential (mV) 0 to 400 0 –100 to 300 0
Pulse height (mV) 25 to 125 50 25 to 125 25
Pulse width (msec) 25 to 125 50 25 to 125 50
Scan increment (mV) 2 to 10 4 2 to 20 4
Scan rate (mV/sec) 10 to 60 50 10 to 100 50
Stirring rate (rpm) 50 to 250 250 50 to 250 250
Rest period (Sec) 2 to 10 5 2 to 10 5
Table 2. DPSV behaviour of analgesic drugs on modified GCE.
Electrode Range studying in g/mL LOD in g/mL % RSD value
Ppy/GCE 0.05 to 0.4 0.035 3.1
PEDOT/GCE 0.025 to 0.4 0.016 2.3
y = 0.0695x - 0.7495
R
2
= 0.9914
y = 0.08x + 2.776
R
2
= 0.9951
0
5
10
15
20
25
30
35
40
0100 200300 400
Conc. (ppb)
ip(A)
Ppy
PEDOT
Figure 6. Calibration plot of DPSV.
antihistamine was compared with that reported already
and the details are presented in Table 3. The table shows
that the differential pulse stripping voltammetry (DPSV)
method using polypyrrole and poly (3,4-ethylenedioxyth-
iophene) modified electrode for the determination of the
analgesics is superior to the already available methods.
3.5. Analysis of Pharmaceutical and Urine
Samples
The pharmaceutical samples having PA was collected
from medical shops at Karaikudi and analyzed. The tab-
lets were powdered, dissolved and subsequently diluted
to a required concentration. DPSV of the drug at pH 13.0
was recorded under optimum experimental conditions.
By substituting the peak current in the calibration plot
and keeping dilution factor in to consideration, the
amount of PA present in the tablet was determined. The
amount of PA determined was 47 ± 0.8 mg from nano
Ppy/GCE and 49 ± 0.5 mg from nano PEDOT/GCE.
These values are in good agreement with the company
reported value, 50 mg.
Measurement of PA in urine samples collected after 8
hours of administration was made. 1.0 ml of the urine
sample was mixed with pH 13.0. This experiment was
repeated for 5 times and the average weight of PA in 1.0
ml of urine sample was determined to be 0.21 g for PA
with relative standard deviation 3.2. There is no appre-
ciable interference due to the presence of small amount
urine present in the electrolyte hence the same calibration
plot was used. There was no degradation of the analyte in
solution during experiment. The other matters present in
tablets and urine samples are not interfering with the
study. This method is simple and suitable for the deter-
mination of PA. Repetition rate is found to be high.
4. Conclusions
Pheniramine maleate, an antihistamine, was anodically
oxidised irreversibly on glassy carbon electrode in the
pH range 1.0 to 13.0 and the oxidation was diffusion
controlled adsorption. The standard rate constant was
also calculated. Effect of pH leads to the conclusion that
pH 13.0 was suitable for analytical studies. Employing
DPSV technique, the adsorptive stripping voltammetric
studies of PA was carried out. Optimum conditions were
arrived at and the influence of concentration was found
out. A calibration plot was made and proposed for the
determination of PA. This was used to find out the
amount of drug present in the pharmaceutical tablet and
urine samples. Lower limit of detection was determined
and the % of RSD confirmed reproducibility of the
method. This method is simple, easy to perform and can
very well be used in the determination of PA in real
samples. Thus stripping voltammetry provides a better
method for the determination of PA over spectral and
other methods.

A Study on Preparation and Use of Nano Poly Pyrrole and Nano Poly(3,4-Ethylenedioxythiophene) Coated Glassy Carbon 962
Electrode for the Determination of Antihistamine in Pharmaceutical and Urine Sample
Table 3. Comparison of available methods.
Methods LOD in μg·mL−1
Gas chromatography-mass spectrometry [29] 2
HPLC method [14] 5 - 50
Capillary isotachophoresis [15 ]
Capillary electrophoresis determination[30]
1,
4 - 28
Micellar liquid chromatography [31] 1
Spectrophotometric determination [32] 9.75 - 32.5
5. Acknowledgments
C. Vedhi, gratefully acknowledge DST for financial
support through Fast Track Scheme for Young Scientists,
New Delhi, India to present this aper.
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