Applied Physics A (2024) 130:287

https://doi.org/10.1007/s00339-024-07422-w

Biomass nanoarchitectonics using an agro waste extract for biological

performance of samarium doped zinc oxide nanoparticles
J. Jothisha1 · Anitha Rexalin Devaraj2 · A. Saranya3 · M. Shandhiya1 · B. Janarthanan1 · M. Ramesh Prabhu4 ·
Z. Mohamed Riyas4 · S. Sharmila3

Received: 3 November 2023 / Accepted: 29 February 2024

© The Author(s), under exclusive licence to Springer-Verlag GmbH Germany, part of Springer Nature 2024

Abstract
The use of trash from agricultural waste materials has been acknowledged as a feasible substitute for producing nanoparticles
in an economical and sustainable manner. In the present study, an agro-waste Limonia acidissima shell extract was used in
synthesizing pure and rare earth (Samarium) doped Zinc Oxide nanoparticles. XRD, FT-IR, SEM, TEM, SAED, and UV–Vis
spectroscopic analysis examine the crystal structure, surface morphology and size, and optical properties of the prepared
nanomaterials. The surface defects and oxygen vacancies were examined from the photoluminescence spectrum (PL). The
oxidation state of Zn (2p), O (1 s) and Sm (3 d) was confirmed from XPS studies. The antibacterial performance of pure
and doped ZnO NPs was evaluated against two pathogens: Pseudomonas aeruginosa and Streptococcus oralis, by agar well
diffusion method at different concentrations with amoxicillin as a positive control. Besides, the DPPH radical scavenging
activity was calculated as 91.15% (ZW) and 82.15% (ZSW) at 500 μg/mL. These results strongly endorse the potential of
Sm-doped ZnO as a new biocidal agent for clinical and healthcare applications.

* S. Sharmila
ssharmilaphy@gmail.com
1
Department of Physics, Karpagam Academy of Higher
Education, Coimbatore, India
2
Department of Physics, AMET University, Chennai, India
3
Department of Physics, Vel Tech Rangarajan Dr Sagunthala
R&D Institute of Science and Technology, Chennai, India
4
School of Physics, Alagappa University, Karaikudi, India

Vol.:(0123456789)
287 Page 2 of 15 J. Jothisha et al.

Graphical Abstract

Limonia
acidissima

Nanoparticles
Zinc nitrate
hexahydrate

ZW
100
ZSW
Limonia

Percentage of inhibition (%)

acidissima 80

shell extract
Zn-O 60

40

20

0
10 50 100 250 500 Ascorbic acid
Concentration(µg/ml)

Keywords Limonia acidissima shell · Sm doped ZnO · Streptococcus oralis · Anti-oxidant

1 Introduction
Nanoparticles (NPs) stand out in a variety of consumer
goods, including food, cosmetics, textiles, health care prod-
ucts, etc. These nanoparticles are also essential for efficient
delivery of medications, waste treatment, biomolecular
detection, and food production [1–8]. It can be prepared
by three distinct methods: physical, chemical or biological
methods. In the earlier methods, it requires the use of haz-
ardous and toxic substances with their byproducts. Due to
unique physicochemical properties, biologically prepared
NPs receive great attention from researchers than bulk mate-
rials, which have been widely employed in medicinal field
especially as drug carrier due to its biocompatible and biode-
gradable nature [3, 4]. Natural extracts (parts of plants) have
the tendency of reducing metal nitrates/ chlorides to nano-
particles. The natural extract is loaded with flavonoids, phe-
nolic compounds, tannins, saponins, proteins which rely as
a reducing and capping agent and plays a major role in con-
trolling the shape and morphology of the particles produced.
Because of their distinct characteristics and potential uses,
transition metal oxide nanoparticles (NiO, M ­ nO2, ­Al2O3,
­TiO2, ­MoO2, ­V2O5, etc.) are receiving increased attention
from researchers. Some of the common procedures used to
create NPs include sol–gel, mechanical milling, combus-
tion, chemical itching, aerosol, and hydrothermal processes
[1, 9, 10].
Due to an intriguing capability as gas sensors, solar cells,
mouthwashes, ointments, surface coating agents, piezoelec-
tric and particularly in biomedical applications, the current
scenario focused on producing zinc oxide nanoparticles
using a various natural extracts in a low cost eco-friendly
way. In addition, this n-type semiconductor exhibits a wide
band gap of 3.37 eV at room temperature. Furthermore, zinc
oxide (ZnO) is a potent metal oxide that filters UV light. The
US FDA recognizes ZnO as safe and uses it in the majority
Biomass nanoarchitectonics using an agro waste extract for biological performance of samarium…
of sunscreen lotions because of its excellent antibacterial,
antifungal, anti-cancer, anti-diabetic, and ability to eliminate
hazardous agents from water [7, 9, 11].
Recently, a significant number of scientists have focused
on using fruits, seeds, roots, leaves, and flowers as bioma-
terials for developing nanoparticles. Aqueous fruit extracts
of Myristica fragrans was employed to prepare ZnO NPs by
S. Faisal et al., [12]. In addition to strong larvicidal action
against mosquitoes (transmit dengue fever), the produced
ZnO-NPs also showed excellent photocatalytic dye degrada-
tion of methylene blue dye in 140 min. The emergence of
MRSA and E. coli as multidrug-resistant bacteria was exhib-
ited by C. Karthikeyan et al., when combining curcumin and
chitosan to prepare ZnO nanomaterial [13]. The product was
able to counteract the bacteriostatic or bactericidal effects
of traditional antibiotics. Antidiabetic and wound healing
property of silver doped ZnO NPs was examined by Y. Iqbal
et al., [14]. Azadirachta indica was utilized as a reducing
agent; Ag doped ZnO NPs exhibit good bio medicinal prop-
erty against E.coli. Dysprosium doped ZnO nano lumino-
phores was reported by R. Kumar and S. K. Mishra via solid
state method [15]. Photo luminescent property of doped ZnO
was examined for different concentration of ­Dy3+ and opti-
mized as 4 wt% exhibit good luminescence activities. Zinc
oxide nanoparticles was reported earlier using extracts of
Nephelium lappaceum L [16], Hibiscus rosa-sinensis L [17],
Fagonia cretica [18], Elaeagnus angustifolia L [19], Corri-
andrum sativum [20], Nerium Oleander [21], Areca catechu
[22], Hibiscus subdariffa L [23], Artocarpus hetrophyllus
[24], Myristica fragrans [25], Acalypha indica [26], Cas-
sia fistula and Melia azadarach [8], Deverra tortuosa [27],
lychee peel [28], Cayratia pedata [29] and so on. Research
on examining the properties of rare-earth (RE) doped ZnO
nanocomposites has been booming recently. The ZnO NPs
that have been REM-doped can be used as fluorescent mark-
ers for biological medical imaging. The photocatalytic and
electrochemical activity of S­ m3+ doped MgO and ZnO nano-
particles were reported by M.R. Anil Kumar using Cicer
artinum as a fuel for combustion method [30]. The elec-
trochemical performance and dye degradation property was
examined against rhodamine-B and malachite green. Under
sunlight, ZnO: ­Sm3+ (1 mol %) exhibit good photocatalytic
activity and MgO: S ­ m3+ showed better EIS properties than
3+
ZnO: ­Sm . A. Sukriti et al., prepared samarium doped zinc
oxide nanoparticles by chemical precipitation method and
analyzed its photoluminescence. Degradation of methylene
blue is 5.38 times higher for Z ­ n0.96Sm0.04O than bare ZnO,
which may be due to more defects and vacancies observed
[31, 32]. D Ranjith Kumar et al., prepared vertically aligned
samarium doped ZnO nanorods by Vapor transport process
[33]. While doping with Sm, the length of the nanorods
decreases identified from FESEM analysis; the photocata-
lytic efficiency improved from 83.02 to 97.3% (6 wt %) for
Page 3 of 15 287
methylene blue in 120 min and decreased to 95.72% for 8
wt % of Sm.
One of the traditional fruits of South India is the wood
apple, or Limonia acidissima, which can be found in Thai-
land, Cambodia, Sri Lanka, and India. Every part of the tree
has therapeutic value. Only 35–50% of the fruit is edible,
and the rest is thrown into the soil as agro-waste [34, 35].
Manavalan Murugan et al., synthesized ZnO NPs using
Limonia acidissima bark, leaves and fruits extract which
showed potentially effect on infected on urinary tract infec-
tions [36]. Hence with above results, the aim of the present
work is focused on preparing pure and rare earth (­ Sm3+)
doped zinc oxide nanoparticles using agro-waste: Limo-
nia acidissima shell extract as the reducing and stabilizing
agent. To the best of our knowledge, preparing Sm doped
ZnO NPs using Limonia acidissima shell extract is reported
for the first time. The role of samarium in modifying the
structural, optical, morphological properties of zinc oxide
nanoparticles and its biological performance (antibacterial
and antioxidant activity) was examined against pathogens
(Pseudomonas aeruginosa and Streptococcus oralis).
2 Experimental and characterization
technique
2.1 Materials
Zinc nitrate hexahydrate (­ ZnNO30.6H2O), samarium nitrate
hexahydrate (Sm(NO3)3. ­6H2O) and ethanol (≥ 99.5%) were
purchased from Sigma Aldrich. Fresh Limonia acidissima
fruit was collected from the local market of Coimbatore,
India.
2.2 Preparation of Limonia acidissima shell extract
The collected fresh Limonia acidissima shell was washed
with distilled water thrice to remove the dust present on
the surface and cut into small pieces. A 25 g of shells are
allowed to boil in 200 mL of distilled water for 15–20 min.
and the resultant solution was filtered using Whatmann No.1
filter paper. The filtrate was used to produce nanoparticles,
and the phytochemicals present in the extract will act as sta-
bilizing and reducing agent.
2.3 Preparation of zinc oxide nanoparticles using
Limonia acidissima shell extract
Zinc nitrate hexahydrate was used as the precursors to pre-
pare zinc oxide nanoparticles. 0.1 M of Zinc nitrate hexa-
hydrate was added to the 100 mL of the shell extract under
constant stirring at 60 °C for 3 h. Once the color of the mix-
ture changed, the solution was transferred to hot plate to dry
287 Page 4 of 15
the mixture. The dried powder was then calcined for 4 h at
400 °C in a muffle furnace. Due to the presence of different
phytochemicals in the extract, the zinc nitrated converted to
zinc oxide nanoparticles. The produced powder will then
be used for characterization. Similarly, for Sm doped ZnO
NPs, 0.098 M of Zinc nitrate hexahydrate and 0.002 M of
samarium nitrate hexahydrate have been employed as the
precursors and above procedure was followed. The final
product was named as ZW (pure) and ZSW (Sm doped) for
further use (Fig. 1).
2.4 Characterization technique
The prαural analysis using X’Pert PRO BRUKER diffrac-
tometer from 10 to 80° using CuK radiation. The functional
group presented was confirmed by Fourier Transform Infra-
red Spectroscopic techniques from wave number ranges
400–4000 ­cm−1. Using a portable laser Raman spectrometer
with an excitation of 785 nm, the phonon vibrational charac-
teristics of the nanoparticles were recorded. Shimadzu- 2450
UV–vis Spectrometer used to learn the optical properties of
the prepared nanoparticles. The sorts of flaws in the material
were determined using Fluoromax Plus C- HORIBA, and
Limonia acidissima shell
Aldehydes
Flavonoids
Zinc Nitrate Hexahydrate
Shell Extract
Fig. 1  Experimental process to synthesis nanoparticles
J. Jothisha et al.
Carl Zeiss are utilized for XPS analysis in a high vacuum
with Al Kα excitation at 250 W. TEM and SAED JEOL JSM
6390 and Tecnai G2 20 S-TWIN used to study the morphol-
ogy of the materials.
2.5 Antibacterial analysis
Through disc diffusion method, the antibacterial activity of
the produced NPs was evaluated against Streptococcus ora-
lis and Psedudomonas aeruginosa which is based on Clini-
cal Laboratory Standard Institute (CLSI) standards [25]. A
100 mL of new culture containing 1 × ­108 CFU ­mL−1 of
bacteria was applied to Mueller Hinton Agar (MHA) plates
using a sterile swab.
Over nutrient agar the bacteria was grown to create its
strain. Sterile filter paper measuring 6 mm in diameter with
samples of 1, 1.5, and 2 mg ­mL−1 concentrations was placed
on the surface of the inoculated agar plate to analyze the bac-
terial stain. It was then incubated for 24 h at 37 °C. Amoxi-
cillin, a common antibiotic -positive control, and DMSO—
negative control. The samples were photo activated under
visible light (2325–2500 lx) for 24 h.
Carbohydrates
Calcination at 400
Glycosides
Samarium Nitrate
Hexahydrate
NPs formation
Biomass nanoarchitectonics using an agro waste extract for biological performance of samarium…
2.6 Antioxidant analysis
In studies on natural product antioxidants, the DPPH test is
frequently used. The idea behind this test is that an antioxidant
is a hydrogen donor. It counts substances that scavenge radi-
cals. At 517 nm (purple), DPPH has a significant absorption
maximum. When an antioxidant absorbs hydrogen, the color
changes from purple to yellow, and DPPH is generated. This
reaction is stoichiometric in terms of the number of hydrogen
atoms absorbed. As a result, the reduction in UV absorption
at 517 nm makes assessing the antioxidant impact simple [38].
Simply prepare a 0.1 mM DPPH solution in methanol
and add 100 μL of it to the sample ZW solution at vari-
ous concentrations (500, 250, 100, 50, and 10 μg/mL). The
components must be swiftly combined and allowed to stand
at room temperature (34 °C) for 30 min. A UV–VIS spec-
trophotometer helps to measure the absorbance at 517 nm.
Ascorbic acid serves as a standard. To calculate the ability
to scavenge the DPPH radical, following formula is used:
DPPH scavenging effect (% inhibition)
= [(absorbance of control
(1)
− absorbance of reaction mixture)
]
∕absorbance of control × 1
3 Results and discussion
3.1 P‑XRD analysis
Figure 2 depicts the XRD pattern of pure and Sm-doped
ZnO NPs. The resulting diffracted peaks correspond to
Fig.2  XRD spectrum of pure (ZW) and Sm doped ZnO (ZSW) NPs
Page 5 of 15 287
(100), (002), (101), (102), (110), (103), (200), (112),
(201), (004), and (202) planes, which coincide with the
JCPDS sheet: 89–1397 with the space group of P63mc
[22, 31]. XRD spectra of ZW show an absence of any other
peaks, indicating the formation of pure zinc oxide. Mean-
while, peaks near 23° for ZSW indicate that few amounts
of samarium did not enter the lattice structure of ZnO,
and the intensity of other peaks also reduced while add-
ing a dopant. The broadening of the rise may be due to
the formation of small nanocrystals. Using Debye-Scherer
equation,
D = k𝜆∕𝛽cos𝜃 (2)
where k-shape factor (0.9), λ-wavelength of X-ray, β-full
width half maximum and θ is the Bragg’s angle, the average
crystallite size was estimated at 21.7 and 25.1 Å for ZW and
ZSW, respectively. Since the ionic radii of Sm (~ 96 pm)
are more significant than that of Zn ions (~ 74 pm), lattice
expansion occurs while adding Sm as a dopant. As a result,
the average crystallite size of ZSW is larger than ZW [32].
Meanwhile, it is smaller than earlier reports of A.Sukriti et
al., and C. Karthikeyan et al., [31, 39]. The crystallite size
and morphology of the nanoparticles are essential param-
eters to enhance biomedical applications [40]. The cell vol-
ume, lattice strain (ε) and defects, such as dislocation density
of the prepared ZnO NPs, are calculated and presented in
Table 1.
The oxygen atoms in the wurtzite structure of ZnO are
arranged in a hexagonal tight pack, with zinc atoms occu-
pying half of the tetrahedral gaps. Tetrahedral coordination
exists for both zinc and oxygen atoms. The computed bond
length between Zn and O atoms matches previous studies
as well as the bond length in the unit cell and adjacent
atoms [41].
3.2 FTIR analysis
FTIR spectrum of the prepared materials is shown in Fig. 3.
Both the materials exhibit a presence of O–H stretching band
due to the water molecule absorbed by the surface at 3441
and 3463 ­cm−1 [43]. Due to the bending mode of water mol-
ecule H–O–H, a weak absorption peak being identified at
1643 and 1656 ­cm−1. The weak peak observed at 1506 ­cm−1
indicates C–C and the presence of carboxylic group ­(COO−)
was confirmed by obtaining a sharp peak at 1384 ­cm−1 [30].
The polysaccharides present in the extract exhibited a char-
acteristic peak of –C–N and –C–O–C stretching vibrations
at 1113 ­cm−1 which is suppressed at ZSW [39]. The weak
Zn–O band observed for ZSW and broad intense peak at 517
and 495 ­cm−1 attributes as stretching band of Zn–O for ZW
 287 Page 6 of 15 J. Jothisha et al.

Table 1  XRD parameter XRD parameters Formula ZW ZSW References

Lattice constant (Å) a=b √

λ 3.2555 3.2384 [32, 41, 42]
3sinθ
c λ 5.2150 5.1855
sinθ
Packing factor c/a 1.6019 1.6012
Cell volume, V (Å)3 47.862 47.095
√
3 2
2
a c
Crystallite size, D (nm) 0.9𝜆 21.744 25.1607
𝛽cos𝜃
Lattice strain, ε 𝛽 0.00451 0.00393
4tan𝜃
Dislocation density, δ (× ­1015) (m)−2 1 2.1155 1.579
D2
Zn–O bond length, L ) 1.9811 1.9798
√ ( ( )2
a2
(Å)
1
3
+ 2
− u c2

a2
where, u = 3c2
+ 0.25

ZSW
789
495
1656

3463
1506
Transmittance (a.u)

1384

ZW

517
1113
3441
1643

1384
4000 3500 3000 2500 2000 1500 1000 500
-1
Wavelength (cm )
Fig. 4  Raman spectrum of pure (ZW) and Sm doped ZnO (ZSW)
NPs
Fig. 3  FTIR spectrum of pure (ZW) and Sm doped ZnO (ZSW) NPs

respectively. This mode is Raman active exclusively. The

and ZSW respectively. Compared to pure, samarium doped
ZnO NPs exhibit a small shift in its wavelength.
3.3 Raman spectroscopy
Raman spectra of ZnO and Sm-doped ZnO nanoparticles
with wavenumber ranging from 300 to 1500 ­cm−1 at room
temperature are shown in Fig. 4. The Raman active zone-
centre for the ZnO wurtzite structure follows representations
(Γ = 1A1 + 2B1 + 1E1 + 2E2) that can be used to express
optical phonons at the Brillouin zone’s G point 14 A. The
B1 mode Raman and infrared inactive mode. To separate
into transverse optical (TO) and longitudinal optical (LO)
phonons, the A1 and E1 modes are polar phonons. The
nonpolar E2 mode contains two frequencies, E 2 (H) and
E 2 (L), connected to oxygen atoms and the Zn sublattice,
Raman spectra have peaks at 450, 1200 ­cm−1, corresponding
to the E2 (H) and E2 (L), respectively. These are the primary
characteristics of the wurtzite ZnO structure, which indicates
good agreement with the XRD analysis. The Sm-doped ZnO
phonon lattice increases the oxygen vaccines to enhance the
ROS mechanism in antibacterial performance [32, 44, 45].
3.4 UV‑DRS analysis
The optical properties of the pure and Sm-doped ZnO NPs
are examined via UV–Vis spectra. Figure 5a illustrates the
absorbance spectrum of the material recorded between 200
and 700 nm. Due to the transfer of electrons from the valence
band to the conduction band of prepared nanoparticles, the
absorption peak was notified at 359 nm. On doping with rare
earth metals, the blue shift occurs (362 nm), possibly due to
Biomass nanoarchitectonics using an agro waste extract for biological performance of samarium… Page 7 of 15 287

ZSW

ZW

b c

Fig. 5  Absorption spectrum (a) and Tauc plot (b,c) of pure (ZW) and Sm doped ZnO (ZSW) NPs

the transfer of charge between f-block electrons and valence
or conduction band [30, 46]. Figure 5b, c depicts Tauc’s plot
of pure and Sm-doped ZnO. Extrapolating the linear portion
of the optical band gap (Eg) can be calculated as 3.08 and
3.15 eV for ZW and ZSW, respectively. The obtained results
are comparable to the literature (3.3 eV). Compared to pure,
rare earth-doped material, it exhibits a slightly higher band
gap, which may be due to the fermi level shift towards the
conduction band. According to the Burstein-Moss effect,
such a shift induces an increase in carrier concentration that
may hinder low-energy transitions [47–49]. The difference in
band gap may also be due to the presence of oxygen vacan-
cies and surface flaws, as confirmed by the PL spectrum.
3.5 Morphological analysis
The surface morphology of the prepared pure and Sm-doped
ZnO NPs was examined using SEM, as shown in Fig. 6. Both
images exhibited nanosized particles with combined spheri-
cal and a few polyhedral shape particles in various sizes.
Compared to Sm-doped ZnO, pure ZnO exhibited smaller
particle sizes, similar to XRD data. The image displayed
a dense, homogeneous morphology without any agglom-
eration. To analyze the size and shape of the nanoparticles,
TEM, and Selected area diffraction pattern (SAED) analysis
were carried out as depicted in Fig. 7a–f. Sm-doped ZnO
NPs have a distinct spherical morphology with well-defined
boundaries and smaller sized particles when compared to
pure ZnO NPs. Particle size is computed, and its histogram
is provided in Fig. 7. Due to the high surface area to vol-
ume ratio, high surface energy results in slight accumula-
tion of the prepared NPs [39]. SAED pattern of pure and
Sm doped ZnO NPs depicts a concentric ring pattern bright
spot implicit in the formation of crystalline natured mate-
rial, and the obtained d-spacing is comparable with that of
XRD results.
287 Page 8 of 15 J. Jothisha et al.

Fig. 6  SEM images of pure (ZW) and Sm doped ZnO (ZSW) NPs

b c
a

6
Count

0
10 15 20 25 30 35 40 45 50
Diameter (nm)

d e f
20

15
Count

10

0
5 10 15 20 25 30 35

Diameter (nm)

Fig. 7  TEM, Histogram and SAED pattern of pure (ZW: a–c) and Sm doped ZnO (ZSW: d–f) NPs

3.6 Photoluminescence’s spectra role. Figure 8 elucidates the PL emission spectra of pure

Photoluminescence spectra (PL) help to locate the defects
present in the prepared material. To enhance the clinical
performance of the nanoparticles, the presence of oxygen
defects and charge carrier separation plays a significant
and Sm-doped ZnO NPs with an excitation wavelength of
325 nm. The emission wavelength was observed at 385, 419,
446 and 468 nm for ZW and 387, 417, 449 and 481 nm for
ZSW, respectively. Due to the direct recombination of the
exciton from the conduction band to the valence band, a
Biomass nanoarchitectonics using an agro waste extract for biological performance of samarium…
Fig. 8  PL emission spectra of pure (ZW) and Sm doped ZnO (ZSW) NPs
near band edge (NBE) was observed at 385 and 387 nm.
At 417 and 419 nm, the violet emission peak appears; due
to oxygen vacancies and irregularities in the structure, an
emission peak is notified at 446 and 449 nm for ZW and
ZSW, respectively [50]. The zinc vacancy (468 nm) present
in ZW disappeared in ZSW, which may be due to the distor-
tion present in the sample. The transition between oxygen
vacancy and interstitial oxygen leads to the emission of a
blue-green band at 481 nm due to the quantum confinement
effect in ZSW [51].
3.7 XPS analysis
X-ray photoelectron spectroscopy (XPS) confirmed the val-
ance states of the prepared Sm-doped ZnO nanoparticle, as
shown in Fig. 9 (a-f). The peaks around 1021, 1045, 1082,
1086.43, 1022, 1044, and 529.59 eV prove the existence
of Zn, Sm, and O, respectively. The line constitutes single
Zn ­2p1/2 and Zn 2­ p3/2 peaks at binding energies of 1021.1
and 1045 eV. Fig. 9a depicts the strong spin–orbit coupling,
which causes the Zn (2p) signal to break into two sym-
metrical peaks, Zn 2­ p1/2 and Zn 2­ p3/2. The peaks at 1021
and 1045 eV for pure ZnO NPs, with a spin–orbit splitting
value of 23 eV, match the discovery of Z ­ n2+ linked to oxy-
gen in the ZnO matrix. From Fig. 9b, the binding energy
values were noted at 1082 and 1086.43 eV, corresponding
to ­Sm3d3/2 and Sm ­3d5/2, respectively. Figure 9c suggested
that Sm present in a valance state of 3 + and 2 + reveals the
confirmation of Sm-doped ZnO. The binding energy values
of 1022 and 1044 eV correspond to peak Zn ­2p1/2, and Sm
­3d5/2 confirms that Sm ions are correctly doped to the ZnO
lattice sites. Figure 9d reveals the oxygen O1s and the cor-
responding binding energy value at 531 eV, respectively. In
Fig. 9e, the survey spectrum of Zn, Sm, and O reveals the
Page 9 of 15 287
formation of Sm-doped ZnO nanoparticles, which may be
suitable for biomedical applications [45, 52, 53].
4 Biomedical application
4.1 Antibacterial and antioxidant activity
Antibacterial and anti-oxidant testing of the nanoparticles
validated their clinical efficacy. Researchers are increas-
ingly focusing on understanding the antibacterial proper-
ties of the nanoparticles. However, the concentration of the
dopant affects the antibacterial effect significantly. Broadly
speaking, a variety of factors, including particle size, com-
posites, dopant concentration, surface-to-volume ratio, par-
ticle morphology, and more, affect biological efficacy. In
the current work, quantum confinement causes blue-green
bands to emerge in the PL spectra of Sm-doped ZnO NPs,
and TEM analysis shows that these NPs contain more tiny
particles than pure ZnO. More ROS were formed by nano-
materials with higher photocatalytic activity and more oxy-
gen vacancies. Specifically, through water splitting in the
cell's cytoplasm, they might have created active free radicals
such singlet oxygen and hydroxide radicals. Singlet oxygen
and hydroxide radicals, or ROS, interact with DNA, lipids,
and other macromolecules found in bacterial cells to disrupt
physiological processes leads to cell death [40].
In the present work, by employing rare earth metals as
a dopant, the antibacterial efficacy of ZnO is boosted. Fig-
ure 10a–f revealed the antibacterial performance of pure and
Sm-doped ZnO NPs by testing the materials against a gram-
positive and gram-negative bacterium: Streptococcus ora-
lis and Pseudomonas aeruginosa, at different concentrations
of 50, 100, 250 and 500 mg/mL. For both bacteria, the zone
287 Page 10 of 15 J. Jothisha et al.

Fig. 9  XPS spectrum of pure (ZW) and Sm doped ZnO (ZSW) NPs a Zn 2p b Sm 3 d c Zn 2p Sm 3 d d O 1 s, e Survey spectrum

of inhibition increased with increasing engagement, and it following mechanism explains formation of free radicals and
was even better than the positive control. The formation of antibacterial activity of Sm doped ZnO [57]:
oxygen vacancies, release of Z­ n2+ ions, size of the particles ZnO + hυ → ­e− + ­h+
and surface defects cause oxidative stress in the cells [40]. It h+ + ­H2O → OH + ­H+
leads to the deformation in the structure and breakdown of e− + ­O2 → ·O2−
the molecules which leads to the cell death. The mechanism O2− + H + → ­HO2·
of reactive oxygen stress is shown in Fig. 10g [54–56]. The HO2· + H + → ­H2O2
Biomass nanoarchitectonics using an agro waste extract for biological performance of samarium… Page 11 of 15 287

Fig. 10  Antibacterial activity of

pure (ZW) and Sm doped ZnO
(ZSW) NPs against Pseu- a b
domonas aeruginosa (a, c, e),
Streptococcus oralis (b, d, f)
and Antibacterial mechanism of
ZnO NPs (g)

c d

18
ZW ZW
14
ZSW e 16 ZSW
f
12 14
Zone of inhibition (mm)

12
Zone of inhibition (mm)

10

10
8

8
6
6

4
4

2 2

0 0
50 100 250 500 PC
50 100 250 500 PC
Concentration (µg/ml) Concentration (µg/ml)

g
 287 Page 12 of 15
ZW
100
ZSW
Percentage of inhibition (%)
80
60
40
20
0
10 50 100
Concentration(µg/ml)
Fig. 11  Antioxidant property of pure (ZW) and Sm doped ZnO
(ZSW) NPs
From the results, it is observed that Sm doped ZnO NPs
is an effective against the pathogen -Pseudomonas aerugi-
nosa at higher concentration which may also increases the
particles’ photoactivity. In the case of Sm doped ZnO NPs,
extra hydroxyl radicals produced by the ­Sm2+ ions activated
­H2O2 and caused cell death after interacting with the cell wall.
Compared to gram-positive bacteria, gram-negative bacteria
exhibit a thin layer of peptidoglycan; which makes the nano-
particles to easily interact with the cell membrane results in
damaging the cells. “Electromagnetic” attraction is developed
between the microorganism (negative charge) and metal oxide
surface (positive charge). As a result, existing exciton will
cause an increase in the concentration of intracellular singlet
oxygen 1O2, a process known as oxidative stress. Due to their
higher internal energy, excited oxygen molecules are more
reactive and thereby increase antibacterial action [58, 59].
Using the DPPH assay, the produced nanoparticles’
antioxidant properties were evaluated. These antioxidants
protect cells from damage by providing an electron to free
radicals and preventing the generation of superoxide, hydro-
gen peroxide, and hydroxyl radicals, known to cause disease
and death. Antioxidants are abundant in fruits and spinach,
which contain various polyphenols and flavonoids and help
to minimize oxidative stress on cells [60]. Most human dis-
orders, including diabetes, cancer, and coronary heart dis-
ease, are treated with flavonoids, which have antioxidative,
antiviral, antibacterial, and antiplatelet properties [61–65].
At lower concentrations samarium doped ZnO exhibit bet-
ter antioxidant property than pure as depicted in Fig. 11.
Pure zinc oxide (ZnO) exhibits good antioxidant properties
at higher concentrations, which are comparable with that of
J. Jothisha et al.
standard ascorbic acid. The prepared Limonia acidissima
shell extract is rich in carbohydrates, flavonoids, sterols,
saponins, glycosides and coumarins, as confirmed by phyto-
chemical analysis which took part in vital role in enhancing
the biological performance of the material.
5 Conclusion
Using the phytochemicals found in Limonia acidissima
shell extract, we prepared pure and Sm-doped ZnO NPs.
The produced nanoparticles exhibit a hexagonal wurtzite
structure in a highly crystalline nature. The typical crystal-
250 500 Ascorbic acid
lite sizes for ZW and ZSW, are 21 and 25 nm respectively,
obtained from Debye–Scherrer formula. The presence of a
weak Zn–O bond and other stretching vibrations is deduced
from FT-IR analysis along with E2 (H) and E2 (L) modes
from Raman spectra. ZSW has a slightly more significant
band gap (3.15 eV) than ZW (3.08 eV) due to a Fermi-level
shift towards the conduction band. The oxidation state of
the molecules was examined from XPS spectra. The pho-
toluminescence spectrum clearly indicates the presence of
zinc, oxygen, and surface defects. The nanoparticles have
good antibacterial properties against human pathogens, par-
ticularly Pseudomonas aeruginosa. Furthermore, they con-
firmed excellent antioxidant activity with a lower I­ C50 of
54.71 μg/mL (ZSW) than ZW (76.97 μg/mL). These results
indicated that employing Limonia acidissima shell extract to
produce nanoparticles (NPs) is an inexpensive and ecologi-
cally friendly option. Furthermore, it was predicted that NPs
of these types will have considerable effects on biomedical
and therapeutic applications in the near future.
Acknowledgements The author (JJ) would like to thank Tamil Nadu
State Council for Science and Technology for providing fund under
Student Project Scheme (PS-003) to complete this work. Dr SS wish
to acknowledge Kalasalingam Academy of Research and Education,
India for extending Raman facility.
Author contributions Jothisha J: Methodology, Financing, Writing –
original draft. Anitha Rexalin Devaraj: validation and formal analysis.
Saranya A: Formal analysis, Investigation. Shandhiya M: Data cura-
tion, Writing – original draft. Janarthanan B: Resources, Data cura-
tion. Ramesh Prabhu M: Writing-review & editing, Data curation.
Mohamed Riyas Z: Formal analysis, Conceptualization. Sharmila
S: Writing-review & editing, Project administration, Supervision and
Data curation.
Data availability All data underlying the results are available as part of
the article and no additional source data are required.
Declarations
Conflict of interest The authors declare that they have no conflict of
interest.
Biomass nanoarchitectonics using an agro waste extract for biological performance of samarium… Page 13 of 15 287

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