Bio-Synthesis of AgNPs and MnNPs of Philodendron giganteum Herbal Extract and catalysis’s activity
Department of Chemistry, Sathaye College (Autonomous), Mumbai - 400057, Maharashtra, India.
*Corresponding Author E-mail: manohar2210@gmail.com
ABSTRACT:
We are presenting our successful bio-synthesis of silver nanoparticles (AgNPs) and manganese nanoparticles (MnNPs) using aqueous extracts from the leaves of P. giganteum, a plant native to India. The aqueous extract from P. giganteum serves as a bio-reductant, facilitating the conversion of Ag⁺ to Ag⁰ during incubation in a dark environment. UV–Vis characterization revealed surface plasmon resonance peaks for AgNPs in the wavelength range of 410–460nm. Scanning electron microscopy energy-dispersive X-ray spectrometry (SEM-EDS) confirmed the agglomeration and spherical shapes of AgNPs and MnNPs with diameters ranging from 18-54nm. The TEM and X-ray diffraction shows that both the nanoparticle is crystalline in nature and AgNPs particles are fcc crystalline in nature. The outstanding catalytic activity of AgNPs was demonstrated by employing the reduction of 4-nitrophenol to 4-aminophenol.
KEYWORDS: P. giganteum Herbal Extract, FTIR, SEM, TEM, EDX, XRD and Catalytic Property.
INTRODUCTION:
Today, we live in an era of Nanoscience and nanotechnology, which plays a significant role across various aspects of life1,2. Nanoscience encompasses the study, manipulation engineering of matter, particles and structures at the nanometre scale-equivalent to one billionth (10⁻⁹m) of a meter3. Among metal nanoparticles, silver nanoparticles (AgNPs) and Manganese nanoparticles (MnNPs) have been extensively studied due to their remarkable properties, including optical, antimicrobial, anticancer and anti-oxidant characteristics. Additionally, they found applications in sensors, catalysis and solar cells4,5.
Various methods can be employed for the synthesis of AgNPs and MnNPs.
The most commonly used approach involves the chemical reduction of Ag+ions from an aqueous solution of silver nitrate, using different reducing agents such as ascorbic acid, hydrazine, ammonium formate, dimethyl formamide and sodium borohydride. However, this chemical reduction method is rapid but toxic, with negative environmental impacts6,7,8. Green synthesis, on the other hand, is eco-friendly, non-toxic and aligns with green chemistry principles. It has become a focus of current nanoscience research. One limitation of phytochemical-mediated nanoparticle synthesis is that it requires longer reaction times compared to conventional chemical reduction methods. To address this, plant-mediated synthesis can be coupled with refluxing the solution at a controlled temperature. This approach ensures pollution-free and eco-friendly chemical transformations, resulting in high yields and ease of processing and handling9,10. Numerous reports in the literature describe the plant-mediated synthesis of nanoparticles using various routes. This approach holds promise for sustainable and efficient nanoparticle production.
In our current study, we report the synthesis of silver nanoparticles (AgNPs) and Manganese nanoparticles (MnNPs) using a simple, rapid, and environmentally friendly approach. We utilize the leaf extract of P. giganteum, a plant found in the regions of Maharashtra, India. Phytochemical screening of the P. giganteum leaf extract reveals its richness in alkaloids, phenols, amino acids, flavonoids, phytosterols, and terpenoids. Notably, the leaf structure exhibits a single layer of palisade cells beneath the upper epidermis. Parenchymatous cells, some containing rosette- and prism-shaped calcium oxalate crystals, fill the space between the collenchymas cells and the vascular bundle11.
The Philodendron species can be found in diverse habitats in tropical America, eastern part of Asia and the West Indies. Most occur in humid tropical forests, but also in swamps, on river banks, roadsides and rock outcroppings. They are shrubs and small trees, most of which are capable of climbing the trunks of other trees with the aid of aerial roots. The P. giganteum has large lobed, deeply cut and feather-like (pinnate) leaves that are borne alternately on the stem. The flowers are at the end of the stem, or in the upper axis of the leaf and the stem. All the parts of the plant are poisonous, due to the presence of calcium oxalate crystals12.
Our investigation aims to explore the potential of P. giganteum leaf extract as both a reducing agent and a stabilizing agent in the synthesis of AgNPs and MnNPs. The use of water in the extraction and reaction medium aligns with green chemistry protocols. Additionally, we assess the catalytic activity of the biosynthesized AgNPs by studying the reduction of 4-nitrophenol to 4-aminophenol in an aqueous medium at room temperature, serving as a model reaction.
MATERIALS AND METHODS:
We used AR grade chemicals available from LOBA Chemicals Mumbai, such as AgNO3 and Mn(NO3)2. The 0.001M solution of both metal ions was prepared in double distilled water.
Preparation of plant extract:
First we washed the leaves with salt water and then with fresh water, dry at room temperature near about five days, these dry leaves were crushed in the mixture. Boiled the crushed leaves in distilled water to reduce the volume of water from 500 cm3 to 200cm3. This extract is cooled at room temperature and filtered with ordinary paper first and finally with Whatman’s filter paper, to get coloured extract.
Preparation of metal ion solution:
We have prepared 0.001M of Ag and Mn solution in double distilled water.
Preparation of Nanoparticles:
We prepared four combinations metal ions with plant extract in the ratios of 1:1, 1:2, 1:3 and 2:1. These solutions are refluxed by using water condenser for four hours in water bath. After completion of four hours, we cooled the solutions and centrifugate at 5000rmp in centrifugate machine near about three hours, to get residue. That residue is dried at room temperature. It is found that these are the nanoparticles of AgNPs and MnNPs. The colour of these solutions before adding the metal solution and after adding the metal solution is shown in figure 1.
Figure 1: Synthesis of Nanoparticles
Figure 2. Nanoparticles with their Characterization Methods
Instrumental method:
Different factors modulate the characteristics of AgNPs like shape, size, crystallinity, surface charge, surface coating, and biological activity. There are several technologies available to study the characters and properties of nanoparticles such as Ultra-violet visible spectroscopy (UV-Vis) spectrophotometer range from 350nm to 800 nm by using spectronic 200 spectrometer, X-ray diffraction (XRD), Fourier Transform Infrared (FTIR) spectroscopy by using the Perkin Elmer spectrophotometer, scanning electron microscopy (SEM), machine used in SEM is Quanta 200 ESEM, Transmission electron microscope (TEM), Dynamic light scattering (DLS) and Atomic Force Microscopy (AFM).
RESULT AND DISCUSSIONS:
FTIR (Fourier Transform Infrared Spectroscopy) is a highly reliable analytical method that detects and displays elements, chemical structures, chemical bonds, functional groups, and bonding arrangements of molecules13,14. Characterization of AgNPs (silver nanoparticles) through FTIR is performed to identify the molecules that act as coating and stabilizing agents, as well as to detect the reduction of silver ions15. The FTIR spectra indicate that amide and carboxylic functional groups may be responsible for the reduction or capping in the green synthesis of AgNPs16. When comparing the IR spectra of plant extract and its metal nanoparticles, the functional group involvement in the biological compounds of the plant extract during the bioreduction of AgNPs is detected through FTIR analysis. Specifically: The peaks observed in the plant extract at 3300–3400 cm⁻¹ correspond to the OH-hydroxyl group of alcohols or phenolic compounds. The absorbance peaks at 3000 and 3050 cm⁻¹ are attributed to the CH bond of an alkane’s functional group in the stretching position of the spectra. The band at 1600–1550 cm⁻¹ represents the amide group due to the carbonyl stretching of proteins. The peaks observed between 1000 and 950 cm⁻¹ correspond to C-N and C-H bending, likely due to phytochemicals such as aromatic and aliphatic amines present in the plant extract. In the case of P. Giganteum extract loaded with greenly synthesized nanoparticles, the FTIR spectrum shows bands at 1745, 1643, 1508, and 1038 cm⁻¹. These bands are assigned to the stretching vibration of C=O bond of carboxylic acid or ester, N-C=O amide bond of proteins, Nitro compounds and C-N amine bond17. Furthermore, the FTIR absorption spectra reveal a sharp absorbance peak at 460 and 630 cm⁻¹, which is characteristic of the Ag-O and Ag-N bonds18. This peak confirms the biosynthesis of AgNPs via phytochemical synthesis, where aldehydes, acids, nitro compounds, amines of polyamines, and hydroxy groups may be present in the plant. Although minor changes were observed at these frequencies, most peaks in the FT-IR spectrum shifted towards lower frequencies and exhibited decreased binding intensity with the nanoparticles. This trend suggests that free carbonyl and NH₂ groups from proteins and amino acid residues have the ability to bind to the metal, possibly forming a protective layer around the nanoparticles.
UV Visible study: We have recorded UV visible spectra from 380- 800nm. It is found that when the concentration changes and time changes the colour of solution will change and so we will get constant UV visible spectra at 410-415nm and 470-475 range. The colour changes observed during AgNPs formation provide valuable insights into the synthesis process. When the solution mixtures transitioned from light yellow to a light apple greenish colour, it indicated the formation of silver nanoparticles19. The absorbance peaks at 410-415nm were observed for the silver nanoparticles and 470nm for MnNPs. These peaks align with the standard silver absorption pattern, consistent with the behaviour of crystalline materials. Notably, when materials are in the nanoscale, their absorption tends to occur at even shorter wavelengths . In summary, the colour changes and UV-vis spectroscopy results provide compelling evidence for the successful formation of silver and manganese nanoparticles, highlighting their unique properties at the nanoscale.
Figure 3: UV–Visible spectra for AgNPs and MnNPs
XRD Analysis study: An X-ray diffractometer was used to analyse a powdered sample of silver nanoparticles structurally. The XRD pattern of biosynthesized silver nanoparticles revealed their highly crystalline structure. As shown in below figure, the bio-fabricated nanoparticles exhibited five distinct peaks corresponding to intensities are 47.7°, 86.6°, 75.4°, 45.5° and 17.2°. the 2θ angles are 28.1,32.8, 38.2,47.1 and 55.5 which matched the (110), (111), (121), (200) and (311) planes respectively. The average crystal size was calculated from the XRD analysis using the Debye–Scherrer equation, which, in this study, was approximately equal to ≈35nm. The data from XRD were compatible with those obtained by SEM analysis. The crystallite domain size was calculated from the width of the XRD peaks, assuming that they are free from non-uniform strains, using the Scherrer formula. D= 0.94 λ / β Cos θ, where D is the average crystallite domain size perpendicular to the reflecting planes, λ is the Xray wavelength, β is the full width at half maximum (FWHM), and θ is the diffraction angle. To eliminate additional instrumental broadening the FWHM was corrected, using the FWHM from a large grained Si sample.
Figure 4. X-ray diffraction pattern of AgNPs
SEM study: Scanning Electron Microscopy (SEM) visualizes the surface morphology of a sample. The image is obtained when electrons are reflected from the sample’s surface. High-resolution SEM images of nanoparticles provide valuable information about their size, shape, topography, composition, electrical conductivity and other properties. Let’s explore example of greenly synthesized AgNPs characterized using SEM: AgNPs synthesized from leaf extract of P. Giganteum. The particle diameter was approximately 18 nm, the images showed the presence of oval and spherical nanoparticles. The AgNPs fell within the range of 18-54 nm and confirmed a face-centered cubic (fcc) crystalline structure of metallic silver. These SEM analyses provide crucial insights into the nanoscale features of AgNPs, aiding in their characterization and potential applications 20,21. This may be due to the availability of different quantity and nature of capping agents present in the leaf extract. EDX spectra recorded from the silver nanoparticles were shown in figure. From EDX spectra, it is clear that silver nanoparticles reduced P. Giganteum have the weight percentage of silver as 61 %.
Figure 5: SEM EDX AgNPs
eZAF Quant Result
|
Element |
Weight% |
MDL |
Atomic% |
Net Int. |
R |
A |
F |
|
C K |
39.* |
0.73 |
65.4 |
211.8 |
0.8535 |
0.1287 |
1.0000 |
|
O K |
20.4 |
0.60 |
26.2 |
125.2 |
0.8671 |
0.0578 |
1.0000 |
|
Al K |
0.10 |
0.14 |
0.10 |
4.30 |
0.8929 |
0.4591 |
1.0100 |
|
Si K |
0.10 |
0.12 |
0.00 |
3.80 |
0.8975 |
0.5806 |
1.0159 |
|
Cl K |
3.50 |
0.19 |
1.90 |
218.2 |
0.9099 |
0.8259 |
1.0502 |
|
Ca K |
2.80 |
0.28 |
1.40 |
100.2 |
0.9213 |
0.7717 |
1.0151 |
|
Ag L |
33.3 |
0.36 |
6.10 |
728.5 |
0.9191 |
0.8572 |
1.0048 |
Figure 6: SEM EDX of MnNPs
eZAF Quant Result
|
Element |
Weight% |
MDL |
Atomic% |
Net Int. |
R |
A |
F |
|
C K |
22.0 |
0.91 |
32.1 |
112.8 |
0.9037 |
0.0661 |
1.0000 |
|
O K |
52.6 |
0.18 |
57.7 |
1597.3 |
0.9144 |
0.1528 |
1.0000 |
|
S K |
9.1 |
1.06 |
5.00 |
1164.8 |
0.9433 |
0.7874 |
1.0135 |
|
K K |
0.1 |
0.09 |
0.10 |
11.2 |
0.9515 |
0.8814 |
1.0448 |
|
Mn K |
16.1 |
0.16 |
5.10 |
736.6 |
0.9660 |
0.9781 |
0.0400 |
Figure 7: TEM Images of AgNPs
Figure 8: TEM Images of MnNPs
Atomic force microscopy (AFM) Study:
AFM is also used for the analysis of size, surface morphology, structural properties and physical characteristics using a phosphorus-doped silicon probe 24. For characterization, the sample of AgNPs is prepared by dissolving it in water or ethanol, and the droplet is applied to the silicon substrate and allowed to dry. After drying, AFM analysis of the silicon substrate, which includes the AgNPs sample is performed using a probe 25. In AFM studies, AgNPs exhibited an average size range of 28.3±2.5nm26.
Zeta potential Study:
Zeta potential analysis is typically conducted to determine the surface charge and stability of a formulation. Through this analysis, one can assess the colloidal stability of AgNPs synthesized using green methods by quantifying the velocity of the nano-sized particles. Under the influence of an electric field, the velocity at which these particles move toward the electrodes is evaluated. Specifically, their zeta potentials were approximately −19.7±0.401 mV, −28.0mV and −31.8±0.7mV, respectively27,28,29. The zeta potential of silver nanoparticles loaded with P. Giganteum extract was analysed, revealing values between approximately −19mV and −25mV. These results indicate that, the AgNPs are relatively stable30.
Dynamic light scattering (DLS) Study:
DLS provides the diameter of particles present in a formulation that is dispersed in a liquid. It determines the size of the colloidal suspension of AgNPs. DLS is based on the principle of light scattering and is widely used for the characterization of AgNPs synthesized using Phytoconstituents31. The dispersed particles in the colloidal suspension scatter light, and as a result, an image of the particles is obtained, allowing the determination of size distribution in the range of 0.3–12 µm. For instance, P. giganteum extract-mediated AgNPs exhibited an average particle size distribution of 32nm32.
Catalytic Property of AgNPs: In our study, we employed the catalytic reduction of 4-nitrophenol (4-NP) with NaBH4 as a model reaction33. Our goal was to investigate the impact of polymeric stabilizers and the influence of reaction temperature on the catalytic performance. The reaction took place in an aqueous phase under mild conditions of pressure and room temperature (25°C). We prepared 4-NP aqueous solutions at a concentration of 0.002M in a 100 cm³ volumetric flask. Next, we prepared a fresh solution of NaBH4 at a concentration of 0.008 M in another 100 cm³ volumetric flask, maintaining a molar ratio of 4-NP to NaBH4 at 1:25. This ratio allowed us to follow a pseudo-first-order kinetic model. Additionally, we prepared a reference NaBH4 solution at a concentration of 0.004 M in a 100 cm³ volumetric flask for UV–Visible measurements. We added 10 mg of the catalyst into a beaker. Then, we added the 4-NP solution. Immediately after, 25 cm³ of NaBH4 solution was added, marking the start of the reaction. After thorough mixing, we withdrew an aliquot from the beaker and transferred it to a quartz cuvette. The cuvette was inserted into the UV–Vis spectrometer’s stage. An induction time of 3.0 minutes was allowed after the NaBH4 addition before starting the measurement. The optical absorbance of the reaction was automatically evaluated every 3.0 minutes for 10 cycles to track the decrease in 4-nitrophenol concentration over time. We conducted similar tests at different temperatures, maintaining the same experimental setup but adjusting the temperatures using the instrument software. This approach allows us to explore the catalytic behaviour of the biosynthesized AgNPs under controlled conditions.
Figure 9: Conversion of 4-NP to 4- Aminophenol
CONCLUSION:
In this study, a simple, ecofriendly and economic biological procedure has been developed to synthesize Ag-NPs and Mn-NPs. The Ag-NPs were synthesized by bio-reduction of silver ions using the brown marine algae P. giganteum aqueous extract. The biosynthesized silver nanoparticles have spherical shapes and the particle size ranges from 18-54 nm with a mean size of 18 nm. The FTIR spectra revealed the involvement of amide and hydroxyl moieties of polysaccharide in the formation of Ag-NPs. The biosynthesized silver nanoparticles are expected to have remarkable applications.
The authors declare no conflict of interest, financial or otherwise.
All authors thank to Principal, HOD, Chemistry of Sathaye College, Mumbai for providing necessary research facility. We also thankful for providing SEM, TEM and EDX facility ICON Labs, Mumbai. FTIR and all other instrumental facilities provided by University of Mumbai.
All are the undergraduate Student except main author all are equally contributed the research work for this paper. All authors have read and agreed to the published version of the manuscript.
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Received on 15.03.2024 Modified on 11.04.2024
Accepted on 23.04.2024 ©Asian Pharma Press All Right Reserved
Asian J. Res. Pharm. Sci. 2024; 14(2):122-128.
DOI: 10.52711/2231-5659.2024.00018