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Synthesis and characterization of chitosan encapsulated nickel oxide

nanoparticles modified with folic acid

Article  in  Materials Today: Proceedings · June 2022

DOI: 10.1016/j.matpr.2022.05.256

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Synthesis and characterization of chitosan encapsulated nickel oxide

nanoparticles modified with folic acid
J. Agnes a,⇑, M.S. Selvakumar b, D. Prem Anand a
a
Materials Research Centre, Department of Physics, St. Xavier’s College (Autonomous), Palayamkottai-627002, Tamilnadu, India1
b
Department of Chemistry, St. Xavier’s College (Autonomous), Palayamkottai-627002, Tamilnadu, India1

a r t i c l e i n f o a b s t r a c t

Article history: This research work was aimed to investigate the physicochemical properties of Chitosan (CS) encapsu-
Available online xxxx lated Nickel oxide (NiO) nanoparticles modified with folic acid (FA), fabricated by a simple solvothermal
method. Characterization of the nanoparticles was carried out using the X-ray diffraction analytical tech-
Keywords: nique. Functional groups were identified by Fourier transform infrared spectroscopy (FTIR). UV–Visible
Folic acid (UV) and Thermogravimetric/differential thermal analyses (TG/DTA) were used to study the optical
Chitosan and thermally decomposed nature of the final products. The crystallite size of the final products using
Nickel oxide
the Debye-Scherrer formula is estimated to be 20.71 nm and 22.29 nm respectively. Tauc’s relation
Zeta potential
has been utilized to estimate the bandgap energy (Eg) of the nanoparticles. A scanning electron micro-
scope (SEM) study was conducted to record the surface structure of the nanoparticles. The observed zeta
potential value of CS-NiO nanoparticles is
20.1 ± 4.12 mV and
16.6 ± 4.18 mV for FA-CS-NiO nanopar-
ticles respectively. Hence, the findings of synthesized nanoparticles could be prioritized to examine the
biological effects in future studies.
Copyright Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of 2022 International Confer-
ence on Recent Advances in Engineering Materials.

1. Introduction hydrothermal interaction of nickel oxide NPs with hemoglobin

Nanostructured transition metal oxide nanoparticles have enor-
mous potential use in optical, catalytic, electrical, magnetic, and
biological applications [1–3]. Advances in the field of nanobiotech-
nology have substantially facilitated the manufacturing of a variety
of metal oxide nanomaterials [4]. NiO thin films produced from
nickel acetate as a starting material are said to show high photo-
catalytic activity in the photo-degradation of [KMnO4] dye. The
nanoparticles (NPs) are uniformly dispersed across the morpholog-
ical surface of this film sample, which is homogeneous nanostruc-
tured [5]. The development of chitosan-based nanoparticles has a
lot of promise as a medicine delivery strategy. Yedi Herdiana
et al. conducted a brief review on the efficiency of chitosan-
based nanoparticles in the treatment of breast cancer by delivering
the medicine to a specific system [6]. Nickel oxide nanoparticles
have piqued attention in a variety of medicinal disciplines. The
⇑ Corresponding author.
E-mail address: cicagnes0@gmail.com (J. Agnes).
1
Affiliated to Manonmaniam Sundaranar University, Abishekapatti-627012, Tir-
unelveli, Tamilnadu, India.
and lymphocytes had no substantial cytotoxicity against lympho-
cytes with lower concentrations. With significant binding affini-
ties, NiO NPs form Van der Waals forces and hydrogen bonds
with Hb residues [7]. The potential of ‘‘Smart” nickel oxide-based
core-shell NPs in photodynamic cancer treatment was discovered
when 30 min of LED panel irradiation resulted in 90% inhibition
[8]. Chitosan is a form of biopolymer that can be found in large
quantities on Earth. Metal-oxide amalgamation has been proposed
as a technique to increase chitosan’s antibacterial characteristics
[9,10]. Hemolytic and cytotoxicity experiments indicated that the
chitosan-coated TiO2 NPs are non-toxic and biocompatible [11].
Folic acid is primarily used as a ligand for the folate receptor, which
is over-expressed on the cell surface of many human cancers and
has a high affinity for it. According to H. N. Nguyen et al., adding
folic acid to the drug delivery system improved cytotoxicity and
cellular absorption in HT29 and Hela cells [12]. V. Gupta et al. com-
pared the antibacterial capabilities of manufactured NiO nanopar-
ticles to bulk NiO and conventional antibiotics in different doses.
He suggested that this research be taken further in the biomedical
field [4]. Nickel oxide nanoparticles were synthesized by different
physical and chemical methods. Among them, Maruthupandy M

https://doi.org/10.1016/j.matpr.2022.05.256
2214-7853/Copyright Ó 2022 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of 2022 International Conference on Recent Advances in Engineering Materials.

Please cite this article as: J. Agnes, M.S. Selvakumar and D. Prem Anand, Synthesis and characterization of chitosan encapsulated nickel oxide nanoparticles
modified with folic acid, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2022.05.256
J. Agnes, M.S. Selvakumar and D. Prem Anand
et al. proposed a chemical reduction method that showed excellent
potential based on biomedical application [13]. The size of nickel
oxide nanoparticles was examined to be between the range of
15 nm to 20 nm. Further, the prime investigation of this work
focused on detecting the presence of 4-acetaminophen in paraceta-
mol and human blood serum samples via a NiO/GCE-based sensor
[14]. Chemically modified chitosan with glycidyl methacrylate
(GMA) nanoparticles were subjected to the magnetic field to find
its effect during the drug delivery. Moreover, the enhanced poten-
tials of folic acid in gastric treatment were determined [15].
Herein, the authors report that the synthesized CS-NiO and FA-
CS-NiO nanoparticles via the solvothermal method were character-
ized by XRD, UV–Visible, FTIR, TG/DTA, SEM, and Zeta potential
analyses. The major goal of this research is to look into the physic-
ochemical properties of Nickel oxide nanoparticles encapsulated
with Folic acid and Chitosan. It is suggested that this effort could
be expanded into the field of biological study.
2. Experimental
2.1. Materials
Nickel Chloride (NiCl26H2O), Chitosan (C6H11NO4)n,
Polyvinylpyrrolidone (C6H9NO)n, and N-hydroxysuccinimide
(NHS) [(CH2CO)2NOH] were supplied from Sigma-Aldrich. Folic
acid (C19H19N7O6) and 1-ethyl-3-(3-dimethylamino propyl)Car-
bodimide (EDC) [C8H17N3], Ammonium hydroxide, Ethylene glycol
(C2H6O2), Diluted Acetic Acid (C2H4O2), Sodium Acetate (CH3-
COONa), Dimethyl Sulphoxide (DMSO) (C2H6OS), and Ethanol
(C2H5OH) were collected from Ponmani chemicals. Without addi-
tional purification, all of the compounds were used.
Fig. 1. Synthesis of (a) CS-NiO NPs; (b) FA-CS-NiO NPs.
2
Materials Today: Proceedings xxx (xxxx) xxx
2.2. Synthesis of CS-NiO nanoparticles
Chitosan- nickel oxide nanoparticles were made using a simple
solvothermal technique. In a 70 mL ethylene glycol solution, 1.50 g
nickel chloride, 0.75 g chitosan, 1.0 g polyvinylpyrrolidone, and
3.6 g sodium acetate were dissolved. A magnetic stirrer was used
to vigorously mix the solution for 5 h. Using a hot air oven, this
combination was heated for 6 h in an autoclave at 300°C. The col-
loidal suspension was then filtered and rinsed with deionized
water and 0.5 percent diluted acetic acid. Finally, the particles
were dried at 60°Celsius in an oven before being collected for fur-
ther processing. Fig. 1. depicts the synthesis process of Chitosan
encapsulated NiO nanoparticles modified with Folic acid.
2.3. Synthesis of CS-NiO NPs modified with folic acid
In a 100 mL DMSO mixture containing 0.2 g CS-NiO NPs, 0.1 g
FA, 0.10 g NHS, and 0.158 g EDC were added. The mixture was
ultrasonicated for 30 min before being agitated overnight using a
magnetic stirrer. To remove the precipitates from the suspension,
filtration was applied (washed with water and ethanol alterna-
tively). FA-CS-NiO nanoparticles were made by collecting the end
products and drying them at 100 °C (6 hrs).
2.4. Characterization
XRD pattern was observed using an X-ray diffractometer, (XRD-
JEOL JDX – 3530) operating with a CuKa radiation source (k = 0.1
5456 nm). FTIR spectra of synthesized nanocomposites were
obtained by Thermo Nicolet, NEXUS between the range of
400 cm
1 – 4000 cm
1. A Jasco UV–Vis spectrophotometer was
J. Agnes, M.S. Selvakumar and D. Prem Anand
Fig. 2. XRD pattern of synthesized (a) CS-NiO NPs, (b) FA-CS-NiO NPs.
used to examine the optical characteristics of the samples over a
wavelength range of 200 nm to 800 nm. TG/DTA analyses were
conducted using SIINT 6300, Japan. The thermal properties of the
nanoparticles were examined in an air atmosphere. A platinum
crucible was used with alpha alumina powder. Scanning electron
microscope (MAKE CARELZEISS, Model: EVO 18) analysis was uti-
lized to obtain the morphology of the nanoparticles. The Zeta Sizer
Nano was used to determine the Zeta potential of the nanoparticles
(Malvern, Coimbatore).
3. Results and discussion
Fig. 2. shows the determined XRD pattern of CS-NiO (2a)
nanoparticles and FA-CS-NiO (2b) nanoparticles in the region of
2h = 10° – 80°. The CS-NiO nanoparticles present several peaks at
2h of 27.1°, 31.4°, 43.2°, 56.1°, 65.8°, and 75°. It has a weak intense
peak at 2h = 27°, which is related to chitosan. The FA-CS NiO
nanoparticles have diffraction peaks at 2h = 31°, 42.6°, 43.6°, and
49.5°. Moreover, the synthesized nanoparticles show crystalline
planes (2 0 0) and (3 1 1) at 2h values of 43° and 75°, which were
identified by JCPDS card no: 0000–047-1049 [16]. The observed
peak at 2h = 31° in high intensity was decreased in the XRD pattern
of FA-CS-NiO NPs. The appearance and disappearance of several
peaks indicate the incorporation of folic acid in the samples. The
peak at 2h = 43.4° corresponds to NiO [17].
The Debye-Scherrer [18] formula has been utilized to estimate
the average crystallite size of resultant products. D = bcoshjk , Where
k (1.5405 Å) is the wavelength of X-ray, b is full width at half max-
imum (FWHM), h is diffraction angle and k is an empirical constant
equal to 0.9. The average crystallite size was found to be 20.71 nm
for CS-NiO nanoparticles and 22.29 nm for FA-CS-NiO
nanoparticles.
To examine the functional groups present in the synthesized
nanoparticles, FTIR analysis was performed. Fig. 3(a) and Fig. 3(b)
reveal the Fourier transform infrared spectra of CS-NiO and FA-
CS-NiO nanoparticles. Both spectra show large absorption peaks
about 3444 cm
1 [19], with weaker peaks at 1633 cm
1, which
are associated with O-H stretching and bending vibrations [20].
The stretching vibration of the nickel oxygen bond is ascribed to
the band located at 617 cm
1 [21]. The stretching bands of the
COO-group are related with spectra around 1419 cm
1 [22]. The
presence of absorption spectra of about 1032 cm
1, and
1119 cm
1 is related to C-O stretching vibration [23]. The charac-
teristic peaks at 2923 cm
1 and 2849 cm
1 correspond to C-H
3
Materials Today: Proceedings xxx (xxxx) xxx
Fig. 3. FTIR spectra of (a) CS-NiO NPs, (b) FA-CS-NiO NPs.
stretching vibrations [24]. The peak near 597 cm
1 is evidence of
the presence of NiO nanoparticles [18].
The UV–Vis spectrum of synthesized nanoparticles is displayed
in Fig. 4. The absorption spectra were recorded between 200 nm
and 900 nm. The efficacy of the NPs depends on several factors
such as particle size and energy gap. The band structure and energy
bandgap of the nanoparticles are the eminent sources in identify-
ing their potential applications. The observed cut-off wavelength
is to be around 250 nm (CS-NiO NPs) and 255 nm (FA-CS-NiO
NPs) respectively. The bandgap energy was calculated using Tauc’s
relation: ðahmÞ = Aðhm
Eg Þ Where a is the absorption coefficient,
n
h is Planck’s constant, A is a constant, m is the photon’s frequency,
and Eg is the bandgap energy. Furthermore, for indirect transitions,
the exponent ’n’ equals 1/2, for direct and allowed transitions,
n = 2, and for forbidden transitions, n = 3/2 [22]. Plotting the linear
extrapolation of (ahv) 1/2 versus hm revealed the bandgap energy.
From Fig. 4b. the estimated optical band gap (Eg) for CS-NiO
nanoparticles is 4.3 eV and 4.6 eV for FA-CS-NiO nanoparticles
[Fig. 4d] respectively.
TG/DTA analysis was used to examine the thermal performance
of the prepared sample. The thermogravimetric curves of produced
nanoparticles are shown in Fig. 5. The determined result [Fig. 5a]
reveals the three stages of weight loss. Initially, there is a gradual
weight loss in the temperature range of 30°C to 128°C and 8 % of
the sample has been decomposed. This is due to the evaporation
of water absorbed by the sample. Secondly, 15 % of mass has been
J. Agnes, M.S. Selvakumar and D. Prem Anand Materials Today: Proceedings xxx (xxxx) xxx

Fig. 4. UV–Vis spectra and Tauc’s plot of CS-NiO NPs (a, b) and FA-CS-NiO NPs (c, d).

Fig. 5. TGA spectra of CS-NiO & FA-CS-NiO NPs (a, c); DTA spectra of CS-NiO & FA-CS-NiO NPs.

lost between 128°C and 557°C. The third stage of weight loss takes
place from 557°C to 786°C.
and approximately 39 % of mass loss has been observed. From
Fig. 5c FA-CS-NiO nanoparticles undergo weight loss in two
steps. The first loss of 11 % in mass occurs from 30 °C to
347 °C. The second weight loss was detected in the temperature
range 347 °C to 741 °C rapidly. There were no considerable
reductions in mass observed above the discussed temperature
ranges. Fig. 5b & 5d show a broad endothermic peak around
690 °C (CS-NiO) and 567 °C (FA-CS-NiO) associated with the
decomposition of organic compounds present in the synthesized
material.

4
J. Agnes, M.S. Selvakumar and D. Prem Anand Materials Today: Proceedings xxx (xxxx) xxx

Fig. 6. SEM images of CS-NiO NPs.

Fig. 7. SEM images of FA-CS-NiO NPs.

Surface morphology of the CS-NiO and FA-CS-NiO nanoparticles
was reported by SEM analysis. Fig. 6 reveals the cubic structure of
CS-NiO NPs in a well-dispersed manner. Few particles are agglom-
erated. On the other hand, the SEM micrographs of FA-CS-NiO NPs
were shown in Fig. 7. The SEM image exhibits the cluster irregular
spherical structure of nanoparticles. The changes observed
between the structures of synthesized nanoparticles indicate the
effective surface modification of nanoparticles.
Zeta potential analysis was carried out for prepared nanoparti-
cles. The zeta potential is used to determine the charge magnitude
of nanoparticles. The presence of high zeta potential in nanoparti-
cles (positive or negative) implies that they are stable. Fig. 8 and

Fig. 8. Zeta potential of CS-NiO NPs. Fig. 9. Zeta potential of FA-CS-NiO NPs.

5
J. Agnes, M.S. Selvakumar and D. Prem Anand
Table 1
Zeta potential value of nanoparticles.
S. No Samples Zeta potential (mV)
1 CS-NiO
20.1 ± 4.12
2 FA-CS-NiO
16.6 ± 4.18
Fig. 9 show the zeta potential of CS-NiO and FA-CS-NiO nanoparti-
cles. The observed zeta potential value of CS-NiO nanoparticles is

20.1 ± 4.12 mV and
16.6 ± 4.18 mV for FA-CS-NiO nanoparticles
respectively. The zeta potential values are presented in Table 1.
These results reveal that CS-NiO and FA-CS-NiO nanoparticles are
moderately stable.
4. Conclusion
In this present study, the author reports the achievement of fab-
ricating chitosan encapsulated NiO nanoparticles modified with
folic acid via the facile solvothermal method. The characterization
studies explore the structure (XRD), functional groups (FTIR), opti-
cal properties (UV–Vis), and thermal behaviour (TG/DTA) of syn-
thesized nanoparticles. The determined average crystallite size is
to be 20.71 nm for CS-NiO nanoparticles and 22.29 nm for FA-
CS-NiO nanoparticles. The observed bandgap energy for CS-NiO
nanoparticles is 4.3 eV and 4.6 eV for FA-CS-NiO nanoparticles.
Moreover, TG/DTA analyses exhibit multistage decompositions
and a broad endothermic peak was detected around 690°C (CS-
NiO) and 567 °C (FA-CS-NiO) respectively. The observed zeta
potential value of CS-NiO nanoparticles is
20.1 ± 4.12 mV and

16.6 ± 4.18 mV for FA-CS-NiO nanoparticles respectively. The
present investigation facilitates that the synthesized nanoparticles
will be a good candidate for biological application.
Declaration of Competing Interest
The authors declare that they have no known competing finan-
cial interests or personal relationships that could have appeared
to influence the work reported in this paper.
Acknowledgement
The authors thank Dr. D. Prem Anand for his assistance in com-
pleting this work.
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