The current study describes the plant-mediated synthesis of lead oxide nanoparticles using a plant extract from Chinese Mahogany. The prepared nanoparticles were characterized using techniques like Fourier transform infrared spectrogram (FTIR), X-ray diffractometer (XRD), field emission scanning electron microscope (FESEM), high resolution transmission electron microscope (HRTEM) and thermo-gravimetric analysis (TGA). XRD results confirmed the crystalline nature of the nanoparticles. The Chinese Mahogany plant extract-lead oxide (CMPE@LO) nanoparticles were used to evaluate photocatalytic behavior against fast green (FG). It was observed that 90.22 % of fast green (FG) has been removed within 3 hours. The various operating parameters such as effect of time, concentration of fast green and photo catalyst amount were also studied and optimized for maximum removal. The kinetic study was investigated using pseudo-first model having good value of regression coefficient (R2). The antibacterial properties of the prepared nanoparticle against several bacteria including B. subtilis, S. aureus, and E. coli, were also investigated. The synthesized CMPE@LO nanoparticles shows higher zone of inhibition as compared to inorganic or organic moiety.
Research Article
Bio-synthesis of lead oxide nanoparticles using Chinese Mahogany plant extract (CMPE@LO) for photocatalytic and antimicrobial activities
https://doi.org/10.21203/rs.3.rs-2490360/v1
This work is licensed under a CC BY 4.0 License
Journal Publication
published 19 Jul, 2023
You are reading this latest preprint version
Chinese Mahogany
lead oxide
photo-catalyst
antimicrobial activity
fast green
A developing area of material science is the synthesis of metal-nanoparticles using plant extracts. Compared to traditional preparation techniques, these are a great replacement because they are affordable, economical and effective [1]. Many technical and environmental challenges, including as the conversion of solar energy, medicine and wastewater treatment can be addressed with the help of these nanomaterials. The quality of drinking water has been declined due to human activity and technological advancement, as is well known given the current state of the environment. The textile industry is a major contributor to the economies of many countries worldwide. These industries produce the more or less colored effluents depending on the degree of fixing of the dyestuffs on the substrates, which varies with the nature of the substances, the intended intensity of colour and the application technique [2].
Aquatic life may get poisoned if this colored water is dumped into receiving water. The dyes disrupt the biological processes in the water system [3]. They pose a problem because in addition to disturbing other human organs like kidney, reproductive, liver, brain and central nervous system, they may be mutagenic and carcinogenic, which cause significant harm to humans. Hence, treatment of dye-based effluents is considered to be most challenging for the environmental fraternity and the industries. Various treatment methods including, physical, physico-chemical and chemical processes have been investigated for treating dye bearing effluents [4].
New techniques and materials are being discovered by researchers as means of transforming wastewater into a useful resource for daily usage. Due to their complex physical, chemical and structural features, bio-nanomaterials are now popular nowadays [5–10]. Bio-nanomaterials are produced from different biological elements like bacteria, fungi, plants, peptides, nucleic acids, etc. Plants contain biomolecules such as proteins, carbohydrates and coenzyme has excellent potential to reduce metal salt into nanoparticles. Firstly, gold and silver metal nanoparticles were explored in the synthesis of nanoparticles using plant extract. A number of metals like Zn, Cu, Sn, Ti and Pb etc. have been used for the synthesis of nanoparticles. These metal nanoparticles offer various applications such as catalysis, antimicrobial and antibacterial activity, sensors, biomedicine etc. [11–17]
Different types of plants such as Aloe barbadensis Miller, Avena sativa, Medicago sativa, Osimum sanctum, Citrus limon, Azadirachta indica, Coriandrum sativum, and Cymbopogon flexuosus etc. has been explored for the nanoparticles synthesis. In this research paper, we had synthesized lead oxide nanoparticles using Chinese Mahogany leaf extract. Chinese mahogany is also called toona sinensis, Chinese cedar, Chinese toon, beef and onion plant and red toon. It is a species of Toona native and found in Korea, China, Nepal, northeastern India, Thailand, Malaysia, Myanmar and western Indonesia. It has been used as a natural herbal medicine for thousands years due to its consistent pharmacological effects. It was termed as an herbal medicine in Chinese folk medicine with good detoxifying, anti-inflammatory and hemostatic effects. Edible leaves and young shoots of Chinese mahogany is used as delicious and nutritious food stuff in China and other Southeast Asia countries because it has special onion like flavor, wealth of carotene and vitamins B and C [18–23].
This paper presents the extraction of Chinese Mahogany plant extract, synthesis of lead oxide nanoparticles and Chinese Mahogany plant extract encapsulated lead oxide nanoparticles. Prepared samples were characterized by using different techniques like FTIR, EDX, SEM, TEM, XRD and TGA etc. Nanoparticles is used for the amputation of fast green using photocatalytic activity. The prepared nanocomposite is also explored for the antimicrobial activity.
2.1. Chemicals and plant material
Lead acetate, Ethylenediaminetetraacetic acid (EDTA), Fast green (FG) and NaOH were purchased from Sigma Aldrich Pvt. Ltd. with 99% purity. All chemicals were of analytical grade.
2.2. Preparation of Chinese mahogany plant extract (CMPE)
Chinese mahogany leaves were collected from the local area. These leaves were thoroughly washed with double distilled water several times and dried. Then leaves were cut into small pieces. The extract was prepared by heating the leaves dispersed in distilled water for 2 hours with continuous stirring. The mixture was then allowed to cool and filtered using Whatman filter paper. The obtained extract was collected and stored at 0°C for further use [24].
2.3. Synthesis of lead oxide (LO) and CMPE@LO) nanoparticles
In this method, 0.1 M lead acetate and 0.1 M EDTA solution were prepared in double distilled water. Then, with continuously stirring, add 0.1 M EDTA solution dropwise to the 0.1 M lead acetate solution in the beaker. After that add 1.0 M NaOH solution to make it basic with continuous stirring at 60°C for 2 hrs [25]. After-this, definite amount of Chinese mahogany plant extract slowly added into the above mixture with continuous stirring for 2 hrs. Then, filter the resulting mixture and obtained precipitates were dried at 50°C (Scheme 1). In this way, six different samples of CMPE@LO nanoparticles have been prepared by varying the mixing ratio of lead acetate, EDTA and CMPE [26].
2.4. Photocatalytic activity
Photocatalytic activity of CMPE@LO nanoparticles was studied using degradation of fast green (FG) dyes from water system [27–29]. The initial concentration of dye was taken in fixed quantity and 100 mg of the CMPE@LO was added to form slurry. The slurry was placed in dark for one hour to establish adsorption-desorption equilibrium. Further, the slurry was exposed to sunlight by controlled stirring. The effect of photo-catalysis of CMPE@LO was studied at different time interval. The concentration of dye was analyzed by UV-visible spectrometer at corresponding wavelength. All experiment has been conducted in triplicate and average value has been reported. The percentage degradation of FG was calculated using following formula:
% Degradation = \(\frac{\complement ˳-{\complement }_{t}}{\complement ˳}\)×100 (1)
Where, C◦ and Ct are initial and final concentration of dye at time t = 0 and t = t, respectively.
2.5. Antimicrobial Activity
The antimicrobial susceptibility of the prepared nanoparticles and composite was evaluated against the gram-negative bacteria and gram-positive bacteria. The antimicrobial activity was performed using a modified well diffusion method [30]. To perform the antimicrobial assay, nutrient agar was used to grow the different bacteria. Bacteria pre-culture broth could stand overnight in a rotary shaker at 35–37°C for 16–18 hours. The pre-culture broth was spread over nutrient agar media plates. After spreading, 6mm wells in diameter were created with the help of puncture on the plates. Antimicrobial activity was tested using 100 µl plant extract, nanoparticles and nanocomposite solution (100mg/ml) whereas, 10 µl antibiotic solutions (100mg/ml) was used against pathogenic bacteria. In addition, streptomycin was considered positive control, whereas triple distilled water was used as a negative control. The Petri plates were incubated for 18–24 hrs at 37°Cfor the growth of bacteria. All the tests were performed in triplicate. The diameters of the inhibition zones obtained around the wells were measured in mm using Hi-Media antibiotic zone scale.
Present study illustrates the extraction of Chinese mahogany leaf extract, lead oxide nanoparticles and Chinese mahogany plant extract-PbO (CMPE@LO) nanoparticles. Six different samples of CMPE@LO nanoparticles have been prepared by varying amount of mixing ratio of lead acetate, EDTA and CMPE. Table 1 summarized details of different sample preparation. Sample, S-5 was finalized for further detailed study.
3.1. Characterization techniques
Figure 1 elucidates the FTIR spectra of (a) CMPE (b) LO (c) CMPE@LO. The changes in FTIR peaks of spectra clearly confirmed the formation of CMPE@LO nanoparticles. The broad absorption band has been observed at 3280 cm-1 was due to the O-H stretching vibration [31]. The absorption peaks at 1556 cm-1 and 1397 cm-1 described the bending vibration of N-H and C-H bonds. The stretching frequency at 1017 cm-1 ascribed to the carbonyl & hydroxyl group. Further, peaks appeared at 841 cm-1 and 680 cm-1 corresponds to the Pb-O bonding [32].
The EDX analysis has been shown in the Figure 2(a). This confirm the formation of Chinese mahogany plant extract-PbO (CMPE@LO) nanoparticles. The results indicate the atomic percentage of different elements i.e. Carbon (52.70%), Oxygen (34.10%), Lead (9.13%), Sodium (0.67%) and Nitrogen (3.41%) in the form of peaks (Table 2). The EDX analysis clearly show the presence of Pb, O, Na and C, which confirm the formation of (CMPE@LO) nanoparticles.
Thermogravimetric analysis (TGA) has been performed in order to determine the thermal stability of nanoparticles and its fraction of volatile components by observing the change in weight, which takes place as a sample is heated at a constant rate. Figure 2 (b) shows TGA graph of CMPE@LO nanoparticles. There was small decrease weight loss of 3.23 % was recorded up to 230 °C to 300 °C, it may be due to evaporation or dehydration of adsorbed water molecules on the surface of nanoparticles. Further, there was huge loss in weight (13.52 %) from 300 °C to 460 °C because of decomposition of the material. After that, a small loss of 0.74 % was observed in between 460 °C to 525 °C may be due to change in atmosphere (N2 to O2) or combustion of carbon. may be due to the formation of the metal oxide. In last, 5.87 % weight loss was noticed from 525 oC to 540 °C because of inert inorganic residues of ash filler on glass fibers. After that, there was no change observed upto 700 °C [33].
Figure 3 (a-d) indicates the scanning electron micrographs (FESEM) of lead oxide and CMPE@LO nanoparticles. It has been observed that smooth surface with long rod like particles in random manner. After mixing fixed amount of Chinese mahogany plant extract into lead oxide solution, the entire morphology of nanoparticles transformed as shown in the Figure 3 (c-d). As we can clearly have noticed that, cluster of nanoparticles with rough and spongy surface which can provide appropriate site for the adsorption of contaminants on its surface.
X-ray diffraction (XRD) method was studied to confirm the crystallinity of synthesized nanoparticles. Figure 4 presents the XRD spectra of lead oxide (LO) and CMPE@LO nanoparticles. It was apparent from spectra that there was huge difference in the intensity of peaks of LO after the incorporation of CMPE. The sharp intensity peaks confirmed that LO@CMPE nanoparticles were crystalline in nature. 94.16 % crystallinity of CMPE@LO nanoparticles was observed using formula as given below:
The obtained nanoparticles were analyzed by XRD to determine the crystal structure. The major peaks appeared at 21.136o, 24.695o, 27.195o, 34.1753o, 40.532o, 44.571o, 49.230o and 54.209o with respective planes i.e. 110, 120, 021, 111, 131, 211, 002 and 211. These peaks show semi crystalline nature of the material. Average crystallite size is also studied using Debye-Scherrer equation [34, 35]. It was found to be 22.56 nm.
Transmission electron micrographs (HRTERM) of LO@CMPE nanoparticles were shown in the Figure 5. TEM images confirmed that the size of synthesized materials lies in the nano-range. Images showed that nanoparticles have highly porous surface with different particle shapes.
3.2. Photo degradation of fast green (FG)
The tauc plot of LO and CMPE@LO nanoparticles have been depicted in Figure 6 (a & b). In order to calculate band gap, a suspension of 5 mg of synthesized material has been prepared in ethanol solution. Later, ultra-sonication of 30 minutes has been done and the UV–visible spectrum was obtained. The band gap of LO and CMPE@LO nanoparticles were calculated using tauc equation as given below [36, 37]:
αhν=B (hν− Eg)n (3)
Where, α is absorption coefficient=2.303 A/l, Eg=optical band gap, B=band tailing parameter, hν= photon energy; n=1/2 for direct band gap.
The optical band gap of LO and CMPE@LO nanoparticles was obtained by extrapolating the straight portion of curve between (αhν)2 and hν when α=0. The band gap was observed to be 2.52 eV and 2.70 eV for LO and CMPE@LO nanoparticles.
Photocatalytic process causes the formation of highly reactive O2* and OH* radicals that converts hazardous pollutants into environmental benign products. In the presence of sunlight, photo-catalyst enhance rate of chemical reaction. It is a redox reaction, which takes place on the surface of photo-catalyst carried out by hole (h+) and electron (e-) present on valence and conduction band. As sunlight falls on the surface, holes are generated in valence band and e- in conduction band. These photo-generated e-/h+ pairs result the formation of highly reactive, energetic species like OH* and O2*. These reactive species oxidize or degrade hazardous pollutants and convert into non-toxic products [38]. Scheme 2 shows the proposed mechanism for the degradation of fast green as given below:
Figure 7 (a) illustrates effect of contact time on FG degradation using CMPE@LO nanoparticles, LO & CMPE in altered intervals of time. It has been observed from graph that 90.22 % of FG was degraded by CMPE@LO nanoparticles, whereas LO and CMPE exhibits the degradation rate of 69.55 % and 48.43 % within 180 minutes (3 hrs). It was also noticed that CMPE@LO nanoparticles have higher photo-degradation potential for FG as compared to LO and CMPE. CMPE@LO has higher degradation efficiency as compared to both inorganic and organic parts. It was due to the fact that addition of CMPE into LO increased the surface area of CMPE@LO and provide the more sites for the adsorption of pollutants.
As illustrated in the Figure 7(b), the effect of initial FG concentrations varied from 10 to 60 mg/L. has been investigated using 30 mg dosage of nanoparticles. It has been found that the degradation rate increases with concentration (10 to 30 mg/L). Maximum degradation efficiency of fast green has been recorded to be 43.55 %, 62.22 % and 89.39 % using LO, CMPE and CMPE@LO nanoparticles at 30 mg/L, respectively, respectively. After that, degradation efficiency has been declined. This may be due to the fact that active sites reduced by the absorption of fast green dye onto nanoparticle surface and these active sites required for the degradation of dyes molecules. These active sites were lacking at higher concentration [39-41].
The effect of CMPE, LO and CMPE@LO nanoparticles dosage on different concentration ranged from 20-180 mg/L has been performed. Figure 7 (c) indicates the effect of photo catalysts amount on the degradation efficiency of FG. It was apparent that photo degradation rate increases from 22.34 % (20 mg/L) to 89.84 % (100 mg/L) for CMPE@LO nanoparticles. In the same way, for LO it was found to be 18.19 % (20 mg/L) to 63.91 % (100 mg/L) and 10.01% (20 mg/L) to 43.21 % (100 mg/L) for CMPE. Subsequently, degradation rate gradually decreases with increasing amount of photo catalysts.
Figure 7 (d & e) shows the absorption spectra of FG dye for LO and CMPE@LO nanoparticles with time. It was recorded that intensities of peaks decrease incessantly with irradiation time which confirmed the successful degradation of FG. Figure 7(f) represent the degradation of FG followed by pseudo-first-order kinetics. The degradation kinetics of FG using CMPE@LO nanoparticles, LO and CMPE were fitted to pseudo-first-order kinetics with higher values of rate constant and R2. Their values were presented in the Table 4. This was evident from Table 4 that CMPE@LO nanoparticles have possessed higher value of rate constant (0.0981min-1). This may be due to the synergetic effect between CMPE and LO nanoparticles.
3.3. Antimicrobial Activity
The present study revealed that synthesized nano-composite showed potent antimicrobial activity against gram-positive and gram -negative bacteria. The inhibition zones (in mm) of varying sizes were obtained as mentioned in Table 3 and Figure 8. The positive control showed the different sizes of zone of inhibition against both gram-positive and gram -negative bacteria i.e., B. subtilis (18±0.567 mm), S. aureus (17±0.616 mm) and E. coli (17±0.538) but negative control showed no zone of inhibition. In Figure 8, synthesized CMPE@LO nanoparticles showed highest zone of inhibition as compared to CMPE and PbO nanoparticles against both the both gram-positive and gram -negative bacteria. CMPE@LO can produce the large amount of •OH radicals as compared to LO & CMPE, that attack the CO groups of the peptide linkages of the bacterial cell wall and destruct the cellular components like lipids, proteins and DNA, causing the death of the bacteria [42-44].
3.4. Reusability and stability
The defining characteristics for the practical applicability of CMPE@LO nanoparticles are their reusability and stability. [45]. Reusability of CMPE@LO nanoparticles was tested for five consecutive phases as shown in the Figure 9 (a). The synthesized nanoparticles used for each cycle was separated from the reaction mixture and washed with distilled water. After the fifth cycle, FG's photo-degradation rate was found to have decreased slightly from 92.22 % to 89.43 %. The modest decrease in photo-degradation efficiency may be caused by the adsorption of chemical intermediates on nanoparticle surfaces, which block the active sites and leave no active sites available. Figure 9 (b) shows the FTIR spectrum for CMPE@LO after 5th cycle of reusability. It has been found that there is no major change observed in the absorption spectrum after recycle, which indicates that CMPE@LO nanoparticles possess good stability.
In summary, Chinese mahogany plant extract-PbO(CMPE@LO) nanoparticles was synthesized by mixing definite amount of CMPE in lead oxide. EDX results confirm the formation of nanoparticles with different elemental composition. SEM images indicates that after mixing organic part into lead oxide (LO) moiety, entire surface modified into porous surface. CMPE@LO was used to evaluate photocatalytic behavior for the photo-degradation of FG dye. The CMPE@LO nanoparticles show higher degradation rate of 90.22%, which was higher than other moieties. CMPE@LO nanoparticles also showed highest zone of inhibition as compared to CMPE and PbO nanoparticles against both the both gram-positive and gram-negative bacteria. The current study provides the fresh insight into the development and fabrication of plant mediated efficient nanostructure with prospective applications in waste-water restoration and anti-microbial activities.
Acknowledgment: Authors wish to express their gratitude to Indian Institute of Technology (IIT), Mandi, India for providing the necessary instrumental facility.
Ethical Approval: All authors and co-authors have followed the ethical guidelines prescribed by the Journal
Informed consent: All authors and co-authors have given their consent for publication of manuscript in this journal.
Competing interests: Authors declare no conflict of interest among them.
Authors' contributions:
Dr. Arush Sharma and Dr Ajay Kumar has performed: Software; Supervision; Validation; Visualization; Writing - original draft, Writing – review & editing, Roles/ Writing - original draft; Writing. Dr. Manita Thakur has done Conceptualization; Data curation; Formal analysis; Funding acquisition; Investigation; Methodology; Project administration; Resources. Dr. Manjula and Dr Swati: Writing – review & editing, has attempted review & editing.
Funding: N/A
Availability of data and materials: Data can be made available on request.
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Schemes 1-2 are available in the Supplementary Files section.
Table 1: Different sample preparation of CMPE@LO nanoparticles
|
Sample No. |
Lead Acetate in mL (0.1 M) |
EDTA (0.1 M) in mL |
Chinese mahogany plant extract (CMPE) in mL |
Mixing Ratio (v/v) |
Yield (g)
|
|
S-1 |
50 |
50 |
50 |
1:1:1 |
0.47 |
|
S-2 |
100 |
100 |
50 |
2:2:1 |
0.77 |
|
S-3 |
100 |
50 |
50 |
2:1:1 |
0.45 |
|
S-4 |
50 |
100 |
50 |
1:2:1 |
0.86 |
|
S-5 |
50 |
50 |
100 |
1:1:2 |
1.22 |
|
S-6 |
50 |
100 |
100 |
1:2:2 |
0.89 |
Table 2: Elements percentage in CMPE@LOnanoparticles
|
Element |
Series |
unn. C [wt.%] |
norm. C [wt.%] |
Atom. C [at.%] |
Sigma) [wt.%] |
|
|
Carbon |
K-series |
15.46 |
20.20 |
52.70 |
9.22 |
|
|
Oxygen |
K-series |
13.33 |
17.41 |
34.10 |
8.72 |
|
|
Lead |
M-series |
46.23 |
60.38 |
9.13 |
5.29 |
|
|
Sodium |
K-series |
0.37 |
0.49 |
0.67 |
0.24 |
|
|
Nitrogen |
K-series |
1.17 |
1.52 |
3.41 |
2.33 |
|
|
|
Total: |
76.57 |
100.00 |
100.00 |
|
|
Table 3: Inhibition zones (mm) of green extract, PbO and composite against different pathogenic strains
|
Bacteria |
CMPE |
LO
|
CMPE@LO |
Positive control |
Negative control |
|
B. subtilis |
11.8±0.527 |
13±0.587 |
15.7±0.554 |
18±0.567 |
ND |
|
S. aureus |
12.6±0.569 |
13±0.553 |
15±0.593 |
17±0.616 |
ND |
|
E. coli |
13±0.648 |
12±0.529 |
15±0.584 |
17±0.538 |
ND |
Table 4. Rate constants for photo-degradation of FG dye using CMPE, LO and CMPE@LO nanoparticles.
|
Rate Constant |
CMPE |
LO |
CMPE@LO |
|
K1 (min-1) |
0.0529 |
0.0789 |
0.0981 |
No competing interests reported.
- GraphicalAbstract.png
Graphical Abstract
- Scheme1.png
- Scheme2.png
