Synthesis of vanadium oxide nanoplates for electrochemical detection of amaranth in food samples:
http://dx.doi.org/10.5599/jese.1394 1153
J. Electrochem. Sci. Eng. 12(6) (2022) 1153-1163; http://dx.doi.org/10.5599/jese.1394
Open Access : : ISSN 1847-9286
www.jESE-online.orghttp://www.jese-online.org/
Original scientific paper
Synthesis of vanadium oxide nanoplates for electrochemical
detection of amaranth in food samples
Reza Zaimbashi1,2, Ali Mostafavi1, and Tayebeh Shamspur1
1Department of Chemistry, Shahid Bahonar University of Kerman, Kerman, Iran
2Young Researchers Society, Shahid Bahonar University of Kerman, Kerman, Iran
Corresponding author: amostafavi@uk.ac.ir; Tel/ Fax: +98 3433257433
Received: May 31, 2022; Accepted: July 12, 2022; Published: October 6, 2022
Abstract
Amaranth dye is an organic compound largely used in the food and beverage industries with
potential toxicity effects on humans. In this paper, a new electrochemical sensor used for
the determination of amaranth in foods was reported, where a kind of V2O5 nanoplates
(V2O5-NPs) was employed as electrode modifying materials. The V2O5 nanoplates modified
electrode enhanced its electrochemical signal obviously in the determination of amaranth
in foods and exhibited a wider linear response ranging from 0.1-270.0 µM with a low
detection limit of 0.04 ± 0.001 µM (3Sb/m). This work offers a new route in developing new
electrochemical sensors for the determination of colorant additives and other hazardous
components in foods.
Keywords
Azo dyes; artificial food dyes; differential pulse voltammetry; screen printed electrode
Introduction
The rapid development of the food industry leads to an increasing number of specific products
with a certain shape, colour, taste, smell, texture, etc. Thus, different food additives such as
presservatives, sweeteners, thickeners, and colouring agents are used to improve the organoleptic
properties of the food. Dyes play a special role here, as the food quality and taste are often
associated with its colour. Colorants have been used throughout history, from the ancient ages to
the present days. In ancient times, natural colorants were used to make cave paintings and some
of these can still be found in the Altamira cave (Spain) and Lascaux cave (France). Dyes are
classified into natural and synthetic. Natural dyes are extracted from plant and animal sources by
physical methods. With the great development of science and technology, synthetic dyes are the
foundation of various industries, including food, textile, pharmaceuticals, paper, leather, and
cosmetics owing to their versatile colours, easy preparation, and low costs. Synthetic dyes can be
classified by their chemical structures. The groups of atoms deciding the dye colours are called
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mailto:amostafavi@uk.ac.ir
J. Electrochem. Sci. Eng. 12(6) (2022) 1153-1163 VANADIUM OXIDE NANOPLATE FOR DETECTION OF AMARANTH
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chromophores and auxochromes. The chromophores include azo (-N=N-), carbonyl (-C=O), nitro
(-NO2), methine (-CH =) and quinoid groups [1,2].
Azo dyes form the largest group of artificial food dyes. Synthetic azo dyes such as amaranth,
tartrazine, sunset yellow, brilliant blue etc., are used in most food items to make them more
attractive. When compared with many natural dyes, these offer harmful effects on the human body,
and many of them are suspected carcinogens too. The proposed study is the determination of
water-soluble synthetic food colourant amaranth, (trisodium(4E)-3-oxo-4-[(4-sulfonato-1-
naphthyl) hydrazono] naphthalene-2,7-disulfonate), using voltammetric techniques. Amaranth has
been extensively used in food, textiles, pharmaceuticals, etc. due to its attractive dark red to purple
colour .Therefore, it is very important and indispensable to develop a sensitive, rapid analytical
method for the determination of amaranth in diverse food products [3-6].
There have been numerous investigations to achieve techniques for effective and green
detection of azo dyes [7-9]. The electrochemical methods are showing great attention in studying
analytes redox behaviour, and a high interest in electrochemical methods giving a fast response, low
cost, high sensitivity, and selectivity exists [10-15]. Voltammetry is a technique utilized for the
analysis of compounds that undergo oxidation or reduction. In the voltammetry methods normally
using electrodes such as glassy carbon electrodes (GCE), carbon paste electrodes (CPE), screen
printed electrodes (SPE), along with some modifiers [16-22]. Different modifiers will show different
electrochemical activities [23-28]. SPEs are designed to analyse low sample volumes and include
three electrodes (working, reference and counter electrode) in the same device. SPEs are mass pro-
duced at low cost and are thus disposable. Considering such remarkable advantages, SPEs have
received widespread acceptance in fields of analytical chemistry, including food analysis [29].
In recent years, interests have focused on the use of nanosized materials in various fields [30-
38]. Nanomaterials are applied in the fabrication of electrochemical sensors due to an increased
surface area of the electrodes, facile electron transfers and decreased surface fouling [39-44]. The
vanadium oxide (V2O5), as n-type semi-conducting metal oxide, has impressive features like optical
bandgap energy (2.3 eV), thermo-electric potentials, appreciable chemical, and thermal stability.
Accordingly, the V2O5 has been used for different purposes like electrochemical sensors and lithium-
ion battery [45-47].
Therefore, the current work aimed to employ the stripping voltammetric technique using a
screen-printed electrode modified with V2O5 nanoplates for sensitive, selctive and accurate
detection of amaranth in real specimens.
Experimental
Chemicals and apparatus
The electrochemical measurements were performed with an Autolab potentiostat/galvanostat
(PGSTAT 302N; Eco Chemie: The Netherlands). Moreover, General Purpose Electrochemical System
(GPES) software has been used to control the experimental condition. Notably, the SPE (DropSens;
DRP-110: Spain) involved 3 major sections of the graphite counter electrode, a graphite working
electrode, as well as a silver pseudo-reference electrode. Finally, we employed a Metrohm 710 pH-
meter to measure the pH.
All reagents had an analytical grade. These products have been purchased from Merck
(Darmstadt; Germany).
R. Zaimbashi et al. J. Electrochem. Sci. Eng. 12(6) (2022) 1153-1163
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Orthophosphoric acid was utilized to freshly prepare all needed phosphate buffer solutions
(PBSs), and sodium hydroxide was responsible for adjusting the desired pH values (the pH range
between 2.0 and 9.0).
V2O5 nanoplates synthesis
According to a typical production protocol, the ammonium metavanadate (0.5 g, AMV, from
Sigma-Aldrich) was dispersed in deionized water (50 mL) while magnetic stirring. The solution pH
value was dropwise adjusted to about 2 using nitric acid while stirring continuously at 323 K. The
evaporation of water during stirring resulted in an orange-coloured gel of vanadium complex that
was then dissolved in methanol (20 mL) in a vial and subsequently allowed to age at an ambient
temperature for 24 hours. The change in the gel colour from light to dark orange occurred when it
was left in methanol. Afterward, the resultant product was washed several times with deionized
water prior to the next testing.
Preparing the electrode
The V2O5 nanoplate stock solution in the aqueous solution (1 mL) was prepared through the
dispersion of V2O5 nanoplates (1 mg) under ultra-sonication for half an hour, whereas 5 µl aliquot
of V2O5 nanoplates was cast on carbon working electrode, followed by the solvent evaporation at
the room temperature. The surface areas of V2O5-NP/SPE and the unmodified SPE were obtained
by cyclic voltammetry (CV) using 1 mM K3Fe(CN)6 at various scan rates. Using the Randles-Sevcik
equation for V2O5-NP/SPE, the electrode surface was found to be 0.096 cm2 which was about 3.1
times greater than unmodified SPE. The brief preparation process of the V2O5-NP/SPE for the
determination of amaranth is shown in Scheme 1.
Scheme 1. The schematic preparation of V2O5-NP/SPE for determination of amaranth
E / mV
I
/
A
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Result and discussion
Structure and morphology
The morphology and structure of the prepared sample were then investigated by field-emission
scanning electron microscopy (FE-SEM) (Figure 1). It is observed that V2O5 nanoparticles with plate-
like morphology have grown well. The thicknesses of the V2O5 nanoplates are around 26 nm.
Figure 1. The FE-SEM images of V2O5 nanoplates at different magnifications
The elemental analysis from the energy dispersive X-ray spectroscopy (EDX) measurement is
presented in Figure 2. The EDS spectrum shows peaks corresponding to V (73.6 wt.%) and O
(26.4 wt.%) elements, thereby confirming the successful formation of the V2O5 nanoplates without
any impurities. Also, to investigate the distribution of elements in the V2O5 nanoplates, the
elemental mapping images of V2O5 are shown in Figure 3.
In
te
n
si
ty
,
a
.u
.
Energy, keV
Element Content, wt.%
V 73.6 1.3
O 16.4 1.3
Figure 2. The EDX spectrum of V2O5 nanoplates
R. Zaimbashi et al. J. Electrochem. Sci. Eng. 12(6) (2022) 1153-1163
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Figure 3. The elemental mapping images of V2O5 nanoplates
Electrochemical response of amaranth at different electrodes
The effect pH value of electrolyte solution was investigated by differential pulse voltammograms
(DPV) in 0.1 M phosphate buffer solution (PBS) at the pH range from 2.0 to 9.0 containing 40.0 μM
amaranth on the V2O5-NPs/SPE surface. The oxidation peaks current of amaranth reached a maximum
value at pH 7.0, and therefore PBS with pH 7.0 was chosen as the optimum pH to detect amaranth.
Figure 4 displays the linear sweep voltammograms (LSV) of the amaranth at unmodified SPE (curve
b) and V2O5-NPs/SPE (curve a), with the same concentration of 200.0 μM in 0.1 M PBS (pH 7.0).
Figure 4. Linear sweep voltammograms curves of unmodified SPE (curve b) and V2O5-NP/SPE (curve a) in
0.1 M PBS containing 80.0 μM amaranth; scan rate: 50 mV s-1
The anodic peak potential for the oxidation of amaranth at V2O5-NPs/SPE (curve a) is about 740 mV
compared with 790 mV, for that on the unmodified SPE (curve b). Similarly, when the oxidation of
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amaranth at the V2O5-NPs/SPE (curve a) and unmodified SPE (curve b) are compared, an extensive
enhancement of the anodic peak current at V2O5-NPs/SPE, relative to the value obtained at the
unmodified SPE (curve b), is observed. In other words, the results clearly indicate that the V2O5-NPs
improve amaranth oxidation.
Effect of scan rate on the determination of amaranth at V2O5-NPs/SPE
The influence of the scan rate (ʋ) on the peak currents (Ipa) of amaranth at V2O5-NPs/SPE was
investigated by LSV. Figure 5 shows the voltammetric response of 80.0 μM amaranth at V2O5-NPs/SPE
at different scan rates in the range of 10 to 300 mV s-1. The oxidation peak current of amaranth
increases linearly with increasing scan rate. Linear regression equation was obtained from the plot Ipa
and vs. 1/2 (square root of scan rate) as follows; Ipa = 1.4242 1/2 – 1.7969 (R2 = 0.9991) for the
oxidation process, which indicates that the reaction of amaranth at V2O5-NPs/SPE is diffusion
controlled.
Figure 5. Linear sweep voltammograms of V2O5-NP/SPE in 0.1 M PBS (pH 7.0) containing 80.0 µM amaranth
at various scan rates; 1-7 correspond to 10, 25, 50, 75, 100, 200 and 300 mV s-1, respectively. Inset: variation
of anodic peak current vs. ν1/2
Chronoamperometric analysis
Chronoamperometric measurements of amaranth at V2O5-NPs/SPE were carried out by setting
the working electrode potential at 0.78 V for the various concentrations of amaranth in 0.1 M PBS
(pH 7.0) (Figure 6). For an electroactive material (amaranth in this case) with a diffusion coefficient
of D, the current observed for the electrochemical reaction at the mass transport limited condition
is described by the Cottrell equation. Experimental plots of I vs. t−1/2 were employed, with the best
fits for different concentrations of amaranth (Figure 6A). The slopes of the resulting straight lines
were then plotted vs. amaranth concentration (Figure 6B). From the resulting slope and Cottrell
equation, the mean value of the D was found to be 3.3×10-6 cm2 s-1.
y = 1.4242x + 1.7969
R2 = 0.9991
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t / s
Figure 6. Chronoamperograms
obtained at V2O5-NP/SPE in 0.1 M
PBS at pH of 7.0 for different con-
centrations of amaranth (1-4 refer
to: 0.1, 0.5, 1.1 and 1.5 mM).
A - The I plot versus t-1/2 observed by
chronoamperograms 1-4;
B - The slope plot of the straight line
vs. concentration of amaranth
Calibration curve
Because DPV commonly has a higher sensitivity than CV, the DPV technique was applied for the
quantitative detection of amaranth. Figure 7 shows the differential pulse voltammograms of
amaranth at various concentrations using V2O5-NPs/SPE (Step potential = 0.01 V and pulse
amplitude = 0.025 V). As seen, the oxidation peak currents of amaranth enhance gradually by
increasing its concentration.
Figure 7. DPVs of V2O5-NP/SPE in
0.1 M (pH 7.0) containing different
concentrations of amaranth. Numbers
1–10 correspond to to 0.1, 2.0, 7.0,
15.0, 30.0, 45.0, 70.0, 100.0, 200.0
and 270.0 μM of amaranth. Inset: plot
of the electrocatalytic peak current as
a function of amaranth concentration
in the range of 0.1-270.0 μM
y = 0.071x + 0.8511
R2 = 0.9995
Camaranth dye / M
Camaranth day / mM
y = 6.1181x + 1.598
R2 = 0.999 S
lo
p
e
,
A
s
-1
/2
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The oxidation peak currents (Ipa) show a good linear relationship with the concentrations of ama-
ranth ranging from 0.1 M to 270.0 μM. The linear equation is Ipa = 0.071camaranth + 0.8511 (R2 = 0.9995)
(Figure 7 (inset)). Also, the detection limit, cm, of amaranth was obtained using equation (1)
cm = 3Sb / m (1)
In the equation, m is the slope of the calibration plot (0.071 µA. µM-1) and Sb is the standard
deviation of the blank response which is obtained from 20 replicate measurements of the blank
solution. The limit of detection (LOD) was estimated to be 0.04±0.001 μM. In addition, Table 1 shows
that the V2O5-NPs/SPE can compete with other sensors for the determination of amaranth.
Table 1. Linear range and LOD obtained at the V2O5-NP/SPE for the determination of amaranth compared with
other sensors.
Electrochemical sensor Method Linear range, µM LOD, µM Ref.
Multiwalled carbon nanotube/Gold
electrodes
Differential pulse
voltammetry
1.0–10.0 0.068 [48]
Graphene/TiO2-Ag based
composites/Gold electrodes
Linear sweep
voltammetry
0.3-100.0 0.1 [49]
Ni–Mo-MOF/Screen printed graphite
electrodes
Differential pulse
voltammetry
0.15–500.0 0.05 [50]
Co3O4-CeO2/Graphene nanocomposite
modified electrode
Differential pulse
voltammetry
2.0–96.0 0.1591 [51]
V2O5 nanoplate/ Screen printed
electrodes
Differential pulse
voltammetry
0.1-270.0 0.04 This work
V2O5-NPs/SPE repeatability and stability
The V2O5-NPs/SPE stability was tested by keeping the new sensor in the PBS at the pH value of
7.0 for 15 days, and then the cyclic voltammograms (CVs) were consequently recorded in the
solution consisting of amaranth (20.0 µM) for the comparison with the CVs recorded before
submersion. The peak amaranth oxidation was not altered, whereas the current was reduced in the
signals by 2.8 % compared to the initial responses. This means satisfactory stability of V2O5-NPs/SPE
and antifouling activity of the modified SPE for the amaranth oxidation. Additionally, the resultant
products for the modified SPE were measured by the CV in the absence and presence of amaranth.
At last, the CVs were recorded in the presence of amaranth u after 15 potential cycles at 50 mV s-1,
such that the currents were decreased up to >2.6 % but the peak potential did not alter.
Analytical application
The determination of amaranth in real samples such as apple Juice and water samples was perfor-
med using V2O5-NPs/SPE sensor. The concentration values of amaranth were calculated by the
standard addition method. The results are summarized in Table 2, the recovery is between 96.4 and
104.3 %, and the relative standard deviations (RSDs) are all less than or equal to 3.4 %. The experi-
mental results confirmed that the V2O5-NPs/SPE sensor has a great potential for analytical application.
Table 2. Determining amaranth in real samples by using V2O5-NP/SPE (n=5).
Sample
c / μM
Recovery, % RSD, %
Spiked Found
Apple juice
4.5 4.6 102.2 2.7
5.5 5.3 96.4 3.4
6.5 6.4 98.5 1.8
7.5 7.6 101.3 2.2
R. Zaimbashi et al. J. Electrochem. Sci. Eng. 12(6) (2022) 1153-1163
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Sample
c / μM
Recovery, % RSD, %
Spiked Found
Tap water
5.0 4.9 98.0 3.2
6.0 6.1 101.7 2.1
7.0 7.3 104.3 3.0
8.0 7.9 98.7 1.9
Conclusions
The voltammetric behavior of synthetic food colorant, amaranth, was studied using a V2O5-NP/SPE
in 0.1 M PBS of pH 7.0. A well-defined oxidation peak was obtained for amaranth at 0.730 V with the
modified electrode. The diffusion-controlled oxidation of amaranth at the modified electrode can be
attributed to the electrocatalytic nature of V2O5 nanoplate since the bare electrode has not produced
an electrochemical signal under the same experimental conditions. The oxidation peak current varies
linearly with a concentration in the range from 0.1-270.0 µM with a limit of detection at 0.04±0.001
µM. The diffusion coefficient for amaranth using V2O5-NP/SPE, 3.3×10-6 cm2 s-1 was obtained. The
sensor was successfully employed for the determination of amaranth in different samples.
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@Article{Zaeimbashi2022,
author = {Zaeimbashi, Reza and Mostafavi, Ali and Shamspur, Tayebeh},
journal = {Journal of Electrochemical Science and Engineering},
title = {{Synthesis of vanadium oxide nanoplates for electrochemical detection of amaranth in food samples:}},
year = {2022},
issn = {1847-9286},
month = {oct},
number = {6},
pages = {1153--1163},
volume = {12},
abstract = {Amaranth dye is an organic compound largely used in the food and beverage industries with potential toxicity effects on humans. In this paper, a new electrochemical sensor used for the determination of amaranth in foods was reported, where a kind of V2O5 nanoplates (V2O5-NPs) was employed as electrode modifying materials. The V2O5 nanoplates modified electrode enhanced its electrochemical signal obviously in the determination of amaranth in foods and exhibited a wider linear response ranging from 0.1-270.0 µM with a low detection limit of 0.04 ± 0.001 µM (3Sb/m). This work offers a new route in developing new electrochemical sensors for the determination of colorant additives and other hazardous components in foods.},
doi = {10.5599/JESE.1394},
file = {:D\:/OneDrive/Mendeley Desktop/Zaeimbashi, Mostafavi, Shamspur - 2022 - Synthesis of vanadium oxide nanoplates for electrochemical detection of amaranth in food sample.pdf:pdf;:www/jESE_V12_No6_1153-1163.pdf:PDF},
keywords = {Azo dyes, artificial food dyes, differential pulse voltammetry, screen printed electrode},
publisher = {International Association of Physical Chemists (IAPC)},
url = {https://pub.iapchem.org/ojs/index.php/JESE/article/view/1394},
}