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Materials Today: Proceedings: I. Ngom, B.D. Ngom, J. Sackey, S. Khamlich
Materials Today: Proceedings: I. Ngom, B.D. Ngom, J. Sackey, S. Khamlich
a r t i c l e i n f o a b s t r a c t
Article history: This contribution reports on the biosynthesis of Nanoscaled Zinc oxide nanoparticles (ZnO-NPs) using
Received 2 August 2019 natural extracts from various parts of the Moringa Oleifera as effective chelating agents. More precisely,
Accepted 10 May 2020 natural extracts from flowers, seeds and leaves of Moringa Oleifera as chelating and/or oxidizing/reduc-
Available online xxxx
ing agents of zinc nitrate hexahydrate are reported for the first time in the current literature. The struc-
tural and optical properties of ZnO-NPs obtained by the leaves are slightly different from those obtained
Keywords: with the other extracts. The average crystallite sizes of ZnO-NPs calculated via X-rays diffraction analysis
ZnO
are found to be 13.2, 13.9, and 10.8 nm for ZnO-NPs synthesized by the flowers, seeds, and leaves respec-
Nanoparticles
Moringa Oleifera
tively while the direct band gap values deducted from Tauc approximation are 3.12, 3.18 and 3.25 eV.
Flowers From the photoluminescence analysis at room temperature, a broad band in the visible centered around
Seeds 450 nm is obtained for all the zinc oxide nanoparticles. One major bioactive compound for each solution
Leaves extract was used to propose a mechanism of the reaction of ZnO-NPs formation: L-ascorbic acid for the
leaves, quercetin for the flowers and oleic acid for the seeds.
Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the NANOSMATAFRICA-
2018.
https://doi.org/10.1016/j.matpr.2020.05.323
2214-7853/Ó 2020 Elsevier Ltd. All rights reserved.
Selection and peer-review under responsibility of the scientific committee of the NANOSMATAFRICA-2018.
Please cite this article as: I. Ngom, B. D. Ngom, J. Sackey et al., Biosynthesis of zinc oxide nanoparticles using extracts of Moringa Oleifera: Structural & opti-
cal properties, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.323
2 I. Ngom et al. / Materials Today: Proceedings xxx (xxxx) xxx
reported the synthesis of ZnO NPs using Moringa Oleifera leaves without any further purification. Weight of 1.5 g of this salt was
extract and zinc nitrate hexahydrate as a precursor. The synthe- dissolved in 50 mL of each solution extract. The pH measurements
sized NPs with a particle size between 16 and 20 nm were agglom- of the mixtures give 4.3 for the flowers, 4.06 for the seeds, and 4.43
erated and showed maximum antimicrobial activities against for the leaves. The mixtures were then heated under magnetic stir-
Staphylococcus Aureus, a member of Firmicutes bacteria, of about ring at about 70 °C for 2 h. The mixtures in which precipitates
23.8%. Surendra, T. V. et al [23] used Moringa Oleifera peels and zinc appear were introduced in the oven at 100 °C until they’re
acetate as a precursor to synthesize ZnO nanoparticles with sizes completely dried. XRD analysis of the samples showed that they
between 40 and 45 nm and spherical in shape. are amorphous. Consequently, the dried samples were annealed
Moringa Oleifera is a fast growing tree belonging to the Moringa- in air at 500 °C for 2 h and characterized using different techniques
ceae family known as a single genus family of shrubs and trees. Its (Fig. 1).
different parts such as leaves, flowers, and seeds are used in nutri-
tional, medical, and also in environmental domains. The leaves are 2.3. Characterization techniques
used in the treatment of diabetes, tuberculosis, fever, stomach
aches, ear infections, and skin infections. Although, many authors Structural properties of as-prepared ZnO-NPs were character-
studied the composition of phytochemicals in this tree [24,25]. ized by X-ray diffraction (XRD) using a diffractometer (Bruker
Ghazali, H. M., et al [26] showed that Moringa Oleifera seeds con- AXS D8 Advance) with 2theta/theta geometry operating at 2 theta
tain about 22 to 40% by weight of oil which contains fatty acids values ranging from 30° to 80° with a step size of 0.034° and radi-
such as oleic acid, palmitic acid, stearic acid, arachidic acid, Gallic ation kCuKa1 = 1.54056 Å. X-ray diffraction analysis was carried out
acid. Other bioactive molecules are present in Moringa Oleifera for all the samples before and after the thermal annealing (at
seeds: O-ethyl-4-(a-L-rhamnosyloxy)benzyl carbamate, 4-(a-L- 500 °C for 2 h). Diffuse reflectance spectra were recorded using a
rhamnosyloxy)benzyl isothiocyanate, b-sitosterol, glycerol-1-(-9- Carry 5000 UV–Vis-NIR spectrometer equipped with an integrating
octadecanoate), 3-O-(60 -O-oleoyl-b-D-glucopyranosyl-b-sitosterol, sphere in a wavelength range of 200–2500 nm. Attenuated Total
b-sitosterol-3-O-b-D-glucopyranoside, 4-(a-L-rhamnosyloxy) Reflection-Fourier Transform Infrared spectroscopy (ATR-FTIR)
benzyl glucosinolate, moringyne [26,27]. was performed by using a Thermo-Nicolet 8700 FTIR spectrometer
The flowers of Moringa Oleifera possess broad bioactive com- to identify the functional groups if any in the different samples.
pound such as glucosinolates ((E)-nerolidol, a-terpineol, benzyl
isothiocyanate, 4-hydroxybenzylglucosinolate), phenolic acids (5- 3. Results and discussion
caffeoylquinic acid, 3-caffeoylquinic acid), flavonoids (Quercetin
3-O-rutinoside, Quercetin 3-O-glucoside, Kaempferol 3-O- 3.1. Structural and crystallographic analysis
rutinoside, Kaempferol 3-O-glucoside, Isorhamnetin 3-O-(f-
malonylglucoside)), proteins, free amino acids, vitamin C [28]. Fig. 2 shows the XRD pattern of the various ZnO-NPs obtained
Moringa Oleifera leaves content many bioactive compounds such after annealing at 500 °C for 2 h of the as-prepared compounds.
as flavanol glucoside, benzoïque acid glucosides, benzaldehyde 4- Before the annealing, ZnO-NPs are amorphous compared to the
O-b-glucoside [25]. Some bioactive compounds are common to annealed samples. For the annealed samples at 500 °C for 2 h, the
the seeds, leaves and flowers namely phenols, crude proteins, and eight peaks are indexed to the pure wurtzite (hexagonal) structure
glucosides. Mineral elements such as Mg, K, Ca, P, and S are also of ZnO (JCPDF n° 00-036-1451) which confirm their high crystal-
found in Moringa Oleifera leaves as well as in the flowers [24]. lization. In term of structural ZnO properties, the leaves, the seeds,
To the best of our knowledge, there is no documentation on the and the flowers of Moringa Oleifera give similar results. The reticu-
biosynthesis of ZnO using the three different biomass namely lar planes (hkl) and the corresponding Bragg diffraction angles h,
leaves, seeds and flowers of the Moringa Oleifera. In this paper, the reticular distance, the full width at half maximum and the
and as mentioned previously, we report on the biosynthesis of diameter of the NPs are summarized in Tables 1, 2 and 3 respec-
ZnO nanoparticles using Moringa Oleifera leaves, seeds, and flowers’ tively for ZnO NPs synthesized via flowers, seeds, and leaves of
extracts as effective stabilizing and chelating agents. The effects of Moringa Oleifera. The inter-planer distance was calculated using
the different bioactive compounds present in these natural extracts Bragg’s law given by the following relation;
on structural and optical properties of ZnO NPs are studied.
2dsinh ¼ nk ð1Þ
where n = 1 and k = 1.54056 Å is the wavelength of Cu-K radiation.
2. Experimental details
The ratio Dd/dbulk (where Dd = dexp – dbulk) is negative for (0 0 2)
plane of all the synthesized ZnO, suggesting that flowers, leaves,
2.1. Preparation of the extracts
and seeds of Moringa Oleifera bioactive compounds lead to the con-
traction of c-direction. Contrariwise, this ratio is positive for (1 0 0),
Flowers, leaves, and seeds of Moringa Oleifera were collected at
(1 0 1), (1 0 2), (1 1 0) planes to indicate elongation conditions
Bambey (department located in the center of Senegal) and dried
through the directions comparatively to the bulk ZnO.
under sunny conditions. All the solutions were prepared in the
Using the relation (2) the average values of the lattice parame-
same procedure. 6 g of each powder (flowers, leaves) or crushed
ters haexp i and hcexp i was deducted.
seeds were immersed in 200 mL of deionized H2O and then heated
at about 50 °C during 2 h under a thorough magnetic stirring to 1=2
2 2 2
extract the maximum of bioactive compounds. The mixtures were dhkl ¼ ½4 h þ k þ hk =3a2 þ l =c2 ð2Þ
filtered to remove residual solids. Clear solutions were obtained.
Their pH measured were: pH 5.2 (flowers), 5.64 (seeds), and As indicated in Table 4, the values of the lattice parameters
5.78 (leaves). match well with the bulk values. The ratio ac almost doesn’t depend
to the type of natural extract from Moringa Oleifera. The crystallite
sizes are calculated using the following Debby Scherrer’s relation:
2.2. Biosynthesis of ZnO nanoparticles
0:94k
For the synthesis, zinc nitrate hexahydrate Zn(NO3)26H2O pur- £¼ ð3Þ
chased from Sigma Aldrich (99.99% purity) was used as precursor
DCOSh
Please cite this article as: I. Ngom, B. D. Ngom, J. Sackey et al., Biosynthesis of zinc oxide nanoparticles using extracts of Moringa Oleifera: Structural & opti-
cal properties, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.323
I. Ngom et al. / Materials Today: Proceedings xxx (xxxx) xxx 3
Please cite this article as: I. Ngom, B. D. Ngom, J. Sackey et al., Biosynthesis of zinc oxide nanoparticles using extracts of Moringa Oleifera: Structural & opti-
cal properties, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.323
4 I. Ngom et al. / Materials Today: Proceedings xxx (xxxx) xxx
Table 1
ZnO by Flowers.
hkl hbulk (rad) hexp (rad) dhklðbulkÞ (Å) dhklðexpÞ (Å) Dd=dhklðbulkÞ FWHM (rad) h£i(nm)
Table 2
ZnO by Seeds.
hkl hbulk (rad) hexp (rad) dhklðbulkÞ (Å) dhklðexpÞ (Å) Dd=dhklðbulkÞ FWHM (rad) h£i(nm)
Table 3
ZnO by Leaves.
hkl hbulk (rad) hexp (rad) dhklðbulkÞ (Å) dhklðexpÞ (Å) Dd=dhklðbulkÞ FWHM (rad) h£i(nm)
Table 4 around 3665 cm1 and 2970 cm1 for the annealed ZnO. The peaks
Average lattice parameters.
around 2893 cm1 can be indexed to the stretching bands of the
Average lattice parameters hai(Å) hci(Å) c/a various functional groups (NH2, HO-C=O, C–H, H3C-O) present in
ZnO by Flowers 3.2522 5.2445 1.613 the bioactive compounds of Moringa Oleifera extracts [9]. The peaks
ZnO by Seeds 3.2438 5.2184 1.608 at 1620 cm1 are attributed to the –C=C (aliphatic) stretching
ZnO by Leaves 3.2530 5.2317 1.608 vibrations and H2O bending modes. The peaks at 1390 cm1
ZnO bulk 3.2498 5.2066 1.602
Please cite this article as: I. Ngom, B. D. Ngom, J. Sackey et al., Biosynthesis of zinc oxide nanoparticles using extracts of Moringa Oleifera: Structural & opti-
cal properties, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.323
I. Ngom et al. / Materials Today: Proceedings xxx (xxxx) xxx 5
Fig. 4. Tauc plots (aht)2 versus ht of ZnO synthesized by (a) flowers; (b) seeds; (c) leaves.
Please cite this article as: I. Ngom, B. D. Ngom, J. Sackey et al., Biosynthesis of zinc oxide nanoparticles using extracts of Moringa Oleifera: Structural & opti-
cal properties, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.323
6 I. Ngom et al. / Materials Today: Proceedings xxx (xxxx) xxx
For each extracted solution, one major bioactive compound is extract, a flavonoid (quercetin) for the flowers and a fatty acid
chosen to describe a plausible mechanism of the reaction as shown (oleic acid) for the seeds. In these mechanisms, the nitrate ion ion-
in Fig. 7. A vitamin (L-ascorbic acid) was chosen for the leaves izes the bioactive compounds for the first step and then the result-
Please cite this article as: I. Ngom, B. D. Ngom, J. Sackey et al., Biosynthesis of zinc oxide nanoparticles using extracts of Moringa Oleifera: Structural & opti-
cal properties, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.323
I. Ngom et al. / Materials Today: Proceedings xxx (xxxx) xxx 7
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cal properties, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.323
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Please cite this article as: I. Ngom, B. D. Ngom, J. Sackey et al., Biosynthesis of zinc oxide nanoparticles using extracts of Moringa Oleifera: Structural & opti-
cal properties, Materials Today: Proceedings, https://doi.org/10.1016/j.matpr.2020.05.323