- Email: [email protected]
Plant-extract mediated synthesis of ZnO nanoparticles using Pongamia pinnata and their activity against pathogenic bacteria
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Contents lists available at ScienceDirect
Advanced Powder Technology journal homepage: www.elsevier.com/locate/apt
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Original Research Paper
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Plant-extract mediated synthesis of ZnO nanoparticles using Pongamia pinnata and their activity against pathogenic bacteria
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S. Ambika, M. Sundrarajan ⇑
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Advanced Green Chemistry Lab, Department of Industrial Chemistry, School of Chemical Sciences, Alagappa University, Karaikudi 630 003, Tamil Nadu, India
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a r t i c l e
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Article history: Received 19 December 2014 Received in revised form 5 June 2015 Accepted 1 July 2015 Available online xxxx Keywords: Green synthesis Pongamia pinnata ZnO nanoparticles Cotton Antibacterial activity
a b s t r a c t Bio-mediated synthesis of metal oxide nanoparticles using plant extract is a promising alternative of traditional chemical synthesis. The present study reports the synthesis of ZnO nanoparticles by biological method. Highly stable and hexagonal phase ZnO nanoparticles were synthesized using Pongamia pinnata leaves extract and were characterized by XRD, UV–vis, DLS, SEM, TEM and FT-IR spectroscopy. The synthesized ZnO nanoparticles were confirmed by XRD and FTIR spectra. Morphology studies indicates spherical nature of the ZnO NPs and EDX shows the highly pure ZnO nanoparticles. The antibacterial activity of ZnO nanoparticles and ZnO nanoparticles coated cotton fabric were tested against Staphylococcus aureus (gram positive) and Escherichia coli (gram negative) organisms by agar diffusion method. Finally, the current study has clearly demonstrated that the ZnO NPs are responsible for significant higher antibacterial activities. Therefore, the study reveals an efficient, ecofriendly and simple method for the green synthesis of multifunctional ZnO NPs using green synthetic approach. Ó 2015 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.
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1. Introduction
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Metal oxide nanoparticles have been intensively studied in the past decade. Nanosized materials have been an important in basic and applied sciences. Biological process for nanoparticle synthesis using microorganisms, enzymes, plants and alga have been proposed as feasible ecofriendly alternatives to chemical and physical methods, because they are hazardous and costly [1–4]. The synthesis of metal and metal oxide nanoparticles have attracted considerable attention in physical, chemical, biological, medical, optical, mechanical and engineering sciences because it has a high surface area. The metal oxides have high fraction of atoms and they have responsible for their fascinating properties such as antimicrobial, magnetic, electronic and catalytic activity [5]. Zinc oxide nanoparticles is attracting tremendous attention due to its stimulating properties like wide direct band gap of 3.3 eV at room temperature and high excitation binding energy of 60 meV [6]. Zinc oxide nanoparticles have received considerable attention due to their unique antibacterial, antifungal, UV filtering properties, high catalytic and photochemical activity [7,8]. Furthermore, ZnO nanoparticles strongly resist or prevent a microorganism and some reports show considerable antibacterial activity of CaO, MgO and ZnO [9].
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⇑ Corresponding author. Tel.: +91 94444 96151; fax: +91 04565 225202.
They are attributed to the generation of reactive oxygen species on the surface of these oxides [10]. Plants extracts provide a biological synthesis route of several metallic nanoparticles, which are more eco-friendly and allows a controlled synthesis with well-defined size and shape of nanoparticles [11–13]. To avoid the use of toxic organic solvents and severe reaction conditions for the preparation of nanomaterials. Recently researchers have been discovering the possibilities of preparing nanomaterials in an aqueous medium with the help of stabilizing, capping or hydrolytic agents [14,15]. Pongamia pinnata contains a wide range of biologically active compounds such as being rich in flavonoids, terpenoids, phenols, saponins, alkaloids and vitamins. P. pinnata was chosen because of its functional properties like anti-inflammatory, antioxidant, antifungal, antimicrobial [16], anti-lipidoxidative, anti-diarrhoeal, anti-ulcer, anti-hyperammonic [17]. Furthermore, the importance of usage of natural, renewable and low cost material P. pinnata could able to produce the metal oxide nanoparticles with aqueous medium by avoiding the presence of hazardous substance and toxic solvents. The aim of this work, to investigate the role of the plant extract is displayed in the formation, stabilization of ZnO nanoparticles synthesis. The crystal structure and surface morphology were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmittance electron microscopy (TEM) technique.
E-mail address: [email protected] (M. Sundrarajan). http://dx.doi.org/10.1016/j.apt.2015.07.001 0921-8831/Ó 2015 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.
Please cite this article in press as: S. Ambika, M. Sundrarajan, Plant-extract mediated synthesis of ZnO nanoparticles using Pongamia pinnata and their activity against pathogenic bacteria, Advanced Powder Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.07.001
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The antibacterial activity of the ZnO nanoparticles and ZnO nanoparticles treated cotton fabric were evaluated by agar diffusion method against Escherichia coli and Staphylococcus aureus bacteria.
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2. Materials and methods
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2.1. Materials
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P. pinnata leaves were collected from Karaikudi, Tamil Nadu, India. Zinc nitrate hexahydrate [Zn(NO3)2 6H2O] and citric acid were purchased from Merck, India Pvt. Ltd. Deionised water was used throughout the reaction process.
6% of citric acid as a crosslinking agent. Coating was carried out by pad-dry-cure method [18,19] using the padding mangle at a pressure of 3 psi to get a wet pickup of 100% on weight of fabric. Finally the padded fabric was subjected to air drying and curing at 80 °C and 150 °C for 5 and 3 min respectively.
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2.6. Testing of antibacterial assessment
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2.2. Preparation of extract
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The collected leaves were thoroughly washed with water and dried at 30 °C in dust free condition. Dried leaves were crushed into finest powder. 10 g of the powder were boiled with 50 ml of water and extracted under reflux condition at 100 °C for 2 h. After two hours, the aqueous leaves extract were obtained by filtering the mixture through a Whatmann No. 1 filter paper and either directly used in the synthesis of ZnO nanoparticles and stored at 0 °C for further experiments.
The agar diffusion method is a relatively quick and easily effected semi-quantitative test to determine the antibacterial activity [20]. ZnO nanoparticles (100 lg/ml) and treated cotton fabric were tested against S. aureus (gram positive) and E. coli (gram negative) organisms. The suspension of bacteria was grown in nutrient broth medium. Test organisms were dispersed over the surface of agar plates. A small amount of sample is gently pushed over the center of nutrient agar plate inoculated with bacterial cells from intimate contact of the sample. Plates were incubated at 37 °C for 24 h. The antibacterial activity of ZnO nanoparticles and treated cotton fabric were demonstrated by the diameter of the zone of inhibition developed in and around the sample. A zone of inhibition is the area in which the bacterial growth is stopped or prevented due to the bacteriostatic effect of the compound and it measures the inhibitory effect of compound towards a particular microorganism.
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2.3. Synthesis of zinc oxide nanoparticles
3. Results and discussion
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3.1. XRD analysis
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2.4. Characterization techniques
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X-ray diffraction (XRD) analysis was performed on X-ray diffractometer (PANanlytical X-Pert PRO) operated at 40 kV and 30 mA. The pattern was recorded by Cu Ka radiation with about 1.54060 Å. Scanning rate of 2°/min and a sample interval of 0.02° were employed in the 2h range from 20° to 80° for the determination of crystallinity, purity and size of the nanoparticles. The surface morphology of the nanoparticles was examined by JEOL JSM 6390 Scanning electron microscope (SEM) instrument operated at an accelerating voltage at 10 kV. For energy dispersive X-ray (EDX) analysis, the particles were dried on a carbon coated copper grid and performed on SEM instrument equipped with thermo EDX attachment. The FTIR analysis of the zinc oxide nanoparticles was performed by Perkin Elmer make Model Spectrum RX1 (Range 4000 cm 1 –400 cm 1). The UV–Visible spectrum was recorded using JASCO UV–vis. 530 spectrophotometer. TEM images were obtained with a Tecnai 20 G2 (FEI make) Transmission Electron Microscope.
For the first time, ZnO NPs synthesis was carried out using P. pinnata extract via environmentally benign synthetic method. P. pinnata due to their higher constituents of polyphenols are responsible for the formation of ZnO NPs. In this nanoparticles synthesis, aromatic hydroxyl groups present in P. pinnata extract with zinc ions to form the complex with acidic medium [21]. These complexes undergo direct decomposition at 350 °C and leads to formation ZnO NPs. X-ray diffraction pattern is taken in order to confirm phase and crystallinity of the ZnO nanoparticles. The XRD peaks are reliable with the JCPDS data card 89-1397 of hexagonal [22] zinc oxide nanoparticles is displayed in the Fig. 1. The detected peaks corresponded to the hexagonal phase ZnO nanoparticles are found in the lattice planes (h, l, k) of (1 0 0), (0 0 2), (1 0 1), (1 0 2), (1 1 0), (1 0 3), (1 1 2) and (2 0 1) in the 2h value: 31.74°, 34.40°, 36.22°, 47.54°, 56.55°, 62.85°, 67.93° and 69.03° respectively. The
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About 0.1 M zinc nitrate hexahydrate were mixed with 25 ml of extract under vigorous stirring for two hours. After the completion of the reaction, the formed dirty colored precipitate was allowed to settle for 24 h. The precipitate was separated from the reaction solution by centrifugation at 6000 rpm for 15 min, washed with deionised water repeatedly to remove the impurities and dried in an oven at 80 °C. To the powdered as-synthesized sample was then subjected to calcination in muffle furnace at 350 °C for 3 h. TEM sample preparation: 5 lL of ZnO NPs solution was put on a carbon-coated copper grid and was further dried before transferring to the transmission electron microscope.
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2.5. Coating of cotton fabric with ZnO nanoparticles
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Fine medium weight of 100% woven cotton fabric was used for the treatment of biosynthetic ZnO nanoparticles by direct application system. The cotton fabric cut to a size 12 cm 12 cm was immersed in the solution containing 3% of ZnO nanoparticles and
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Intensity (a.u)
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2 Theta Fig. 1. XRD pattern of ZnO nanoparticles.
Please cite this article in press as: S. Ambika, M. Sundrarajan, Plant-extract mediated synthesis of ZnO nanoparticles using Pongamia pinnata and their activity against pathogenic bacteria, Advanced Powder Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.07.001
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Fig. 3. DLS analysis of ZnO nanoparticles.
Fig. 2. UV–Visible spectrum of ZnO nanoparticles.
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crystallite size of the narrow and strong diffraction peak (1 0 1) was 26 nm, determined by Debye–Scherrer’s equation [23]. The narrow peak confirmed the crystallinity of synthesized ZnO nanoparticles.
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3.2. UV–Visible studies
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UV–visible absorption spectroscopy is widely used technique to examine the optical properties of nanosized particles. Fig. 2 shows the peak at 230 nm wavelengths was observed in the UV–visible spectrum, this result confirmed the presence of ZnO nanoparticles synthesized from the leaf extract of P. pinnata which lie much below the band gap wavelength of 358 nm. Thus, there is a strong blue shift in the absorption spectra of the ZnO nanoparticles is indicating that particles must be smaller than the bohr radius of exciton which is for ZnO [24]. This peak is the characteristic of the ZnO formation while confinement in nano scale is proved by blue shift.
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3.3. DLS analysis
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Dynamic light scattering (DLS) is widely being used to measure the size distribution of the prepared ZnO nanoparticles.
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The resulting particle size of ZnO nanoparticles exhibits the size distribution starting from 10 to 120 nm with maximum size distribution is around 90 nm shown in the Fig. 3. Relatively good symmetry of size distribution diagrams in DLS analysis illustrates uniformity of the formed ZnO nanoparticles.
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3.4. SEM and TEM analysis
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SEM image is employed to predict the morphology of the ZnO nanoparticles. SEM images of ZnO nanoparticles under different magnifications are displayed in Fig. 4. It is observed that most of the nanoparticles are spherical in shape with agglomeration and confirmed the average size of about 100 nm. The boundary of the single nanoparticles cannot be regarded by intense observation of the SEM images. Further analysis of the ZnO nanoparticles by EDX spectrum in Fig. 5 confirmed the signal characteristic of zinc and oxygen only. All the presented peaks are assigned for Zn and O without any unknown signals proves the purity of ZnO nanoparticles by calcination. The morphology and size of ZnO nanoparticles was confirmed by employing TEM analysis with their corresponding SAED pattern is represented in Fig 6. The TEM image of ZnO nanoparticles are dispersed as a maximum nanorod and hexagonal particles morphology and range in size of 100 nm. Therefore, the nanorod adopts the polycrystalline structure.
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Fig. 4. SEM images of ZnO nanoparticles at different magnification.
Please cite this article in press as: S. Ambika, M. Sundrarajan, Plant-extract mediated synthesis of ZnO nanoparticles using Pongamia pinnata and their activity against pathogenic bacteria, Advanced Powder Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.07.001
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Fig. 5. EDX spectrum of ZnO nanoparticles.
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3.5. FT-IR spectroscopy FTIR analysis was performed to determine the functional groups in the synthesis of ZnO NPs. Fig. 7 shows that the FT-IR spectra of ZnO nanoparticles in the 500–4000 cm 1 regions. The broad peak 3403.48 cm 1 was indicate the AOH stretching vibrations. The sharp peak present in the range of 2355.86 cm 1 indicates the free carbonyl group. The peaks at 1714.33 cm 1 is due to the presence of stretching vibrations of C@O bond due to non-ionic carboxylic groups and may be assigned to carboxylic acids or their esters in the natural compound. The band at 1364.80 cm 1 is due to the presence of CAOAH bending mode. It is apparent that the intensity of absorption in the region of 516.52 cm 1 characteristic of hexagonal phase ZnAO vibrations at 350 °C. This suggests that the biological molecules could possibly act as hydrolyzing agent for the metal oxide nanoparticles synthesis.
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3.6. Antibacterial activity of ZnO nanoparticles and treated cotton
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ZnO nanoparticles and treated cotton were tested for its antibacterial activity against the bacterial pathogens, S. aureus (gram positive) and E. coli (gram negative) by agar diffusion method. Zone of inhibition values determined for the treated cotton and ZnO (100 lg/ml) nanoparticles were shown in Table 1. Both treated fabric and ZnO nanoparticles pronounced significant growth inhibitory effect against both bacteria due to their large surface area by their nanosize (Fig. 8). However ZnO nanoparticles treated fabric possess superior antibacterial activity against S. aureus than E. coli bacteria which are clearly visualized in the
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Wavenumber Cm-1 Fig. 7. FT-IR analysis of ZnO nanoparticles.
Table 1 Zone of inhibition (mm) values against test organisms. Samples
Cotton ZnO nanoparticles ZnO nanoparticles treated cotton
Bacterial Pathogens S. aureus
E. coli
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antibacterial photographs. A gram positive bacterium is thick, cell wall consisting mainly of peptidoglycan surrounding the cytoplasmic membrane and gram negative bacterial cell wall more complex than a gram positive cell, both structurally and chemically. The antibacterial activity may be due to the following assumptions: microorganisms like bacteria have a small pore in cell membrane. Reactive oxygen species (ROS) are generated [25] from the ZnO-nanoparticles actively penetrates the cell membrane using pores of the cell. The leakage of proteins, minerals and some matters from the cell because of the ROS penetrate the cell wall. The cell membrane is damaged, so the bacteria are killed or inhibited of cell growth. Therefore, the present finding clearly revealed that the prepared ZnO nanocrystals using P. pinnata extract could be applied to the fabrics is an excellent antimicrobial activity.
Fig. 6. TEM image of ZnO nanoparticles.
Please cite this article in press as: S. Ambika, M. Sundrarajan, Plant-extract mediated synthesis of ZnO nanoparticles using Pongamia pinnata and their activity against pathogenic bacteria, Advanced Powder Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.07.001
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Fig. 8. Antibacterial activity of (a) ZnO nanoparticles (b) ZnO nanoparticles treated cotton against S. aureus (1) and E. coli (2).
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4. Conclusion
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In this study, a simple, ecofriendly and economic biological process has been developed to synthesize hexagonal phase ZnO nanoparticles via greener method using P. pinnata leaves extract. Crystallization, phase are evaluated by XRD exhibit the crystalline in nature at 350 °C. The ZnO nanoparticles growth limited to about 100 nm is resulted by the DLS, TEM and SEM techniques. Antibacterial activity of ZnO nanoparticles exhibit pronounced skill against the pathogenic bacteria. This types of metal oxide nanoparticles successfully minimize the infections with pathogenic bacteria.
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Acknowledgement
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The authors greatly acknowledge the Department of Physics, Alagappa University for providing XRD (DST-FIST) facilities.
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Please cite this article in press as: S. Ambika, M. Sundrarajan, Plant-extract mediated synthesis of ZnO nanoparticles using Pongamia pinnata and their activity against pathogenic bacteria, Advanced Powder Technology (2015), http://dx.doi.org/10.1016/j.apt.2015.07.001
No. of Pages 6, Model 5G
7 July 2015 Advanced Powder Technology xxx (2015) xxx–xxx 1
Contents lists available at ScienceDirect
Advanced Powder Technology journal homepage: www.elsevier.com/locate/apt
2
Original Research Paper
6 4 7 5
Plant-extract mediated synthesis of ZnO nanoparticles using Pongamia pinnata and their activity against pathogenic bacteria
8
S. Ambika, M. Sundrarajan ⇑
9
Advanced Green Chemistry Lab, Department of Industrial Chemistry, School of Chemical Sciences, Alagappa University, Karaikudi 630 003, Tamil Nadu, India
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a r t i c l e
i n f o
Article history: Received 19 December 2014 Received in revised form 5 June 2015 Accepted 1 July 2015 Available online xxxx Keywords: Green synthesis Pongamia pinnata ZnO nanoparticles Cotton Antibacterial activity
a b s t r a c t Bio-mediated synthesis of metal oxide nanoparticles using plant extract is a promising alternative of traditional chemical synthesis. The present study reports the synthesis of ZnO nanoparticles by biological method. Highly stable and hexagonal phase ZnO nanoparticles were synthesized using Pongamia pinnata leaves extract and were characterized by XRD, UV–vis, DLS, SEM, TEM and FT-IR spectroscopy. The synthesized ZnO nanoparticles were confirmed by XRD and FTIR spectra. Morphology studies indicates spherical nature of the ZnO NPs and EDX shows the highly pure ZnO nanoparticles. The antibacterial activity of ZnO nanoparticles and ZnO nanoparticles coated cotton fabric were tested against Staphylococcus aureus (gram positive) and Escherichia coli (gram negative) organisms by agar diffusion method. Finally, the current study has clearly demonstrated that the ZnO NPs are responsible for significant higher antibacterial activities. Therefore, the study reveals an efficient, ecofriendly and simple method for the green synthesis of multifunctional ZnO NPs using green synthetic approach. Ó 2015 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.
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1. Introduction
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Metal oxide nanoparticles have been intensively studied in the past decade. Nanosized materials have been an important in basic and applied sciences. Biological process for nanoparticle synthesis using microorganisms, enzymes, plants and alga have been proposed as feasible ecofriendly alternatives to chemical and physical methods, because they are hazardous and costly [1–4]. The synthesis of metal and metal oxide nanoparticles have attracted considerable attention in physical, chemical, biological, medical, optical, mechanical and engineering sciences because it has a high surface area. The metal oxides have high fraction of atoms and they have responsible for their fascinating properties such as antimicrobial, magnetic, electronic and catalytic activity [5]. Zinc oxide nanoparticles is attracting tremendous attention due to its stimulating properties like wide direct band gap of 3.3 eV at room temperature and high excitation binding energy of 60 meV [6]. Zinc oxide nanoparticles have received considerable attention due to their unique antibacterial, antifungal, UV filtering properties, high catalytic and photochemical activity [7,8]. Furthermore, ZnO nanoparticles strongly resist or prevent a microorganism and some reports show considerable antibacterial activity of CaO, MgO and ZnO [9].
46 47 48 49 50 51 52 53 54 55 56 57 58 59 60 61 62 63 64
⇑ Corresponding author. Tel.: +91 94444 96151; fax: +91 04565 225202.
They are attributed to the generation of reactive oxygen species on the surface of these oxides [10]. Plants extracts provide a biological synthesis route of several metallic nanoparticles, which are more eco-friendly and allows a controlled synthesis with well-defined size and shape of nanoparticles [11–13]. To avoid the use of toxic organic solvents and severe reaction conditions for the preparation of nanomaterials. Recently researchers have been discovering the possibilities of preparing nanomaterials in an aqueous medium with the help of stabilizing, capping or hydrolytic agents [14,15]. Pongamia pinnata contains a wide range of biologically active compounds such as being rich in flavonoids, terpenoids, phenols, saponins, alkaloids and vitamins. P. pinnata was chosen because of its functional properties like anti-inflammatory, antioxidant, antifungal, antimicrobial [16], anti-lipidoxidative, anti-diarrhoeal, anti-ulcer, anti-hyperammonic [17]. Furthermore, the importance of usage of natural, renewable and low cost material P. pinnata could able to produce the metal oxide nanoparticles with aqueous medium by avoiding the presence of hazardous substance and toxic solvents. The aim of this work, to investigate the role of the plant extract is displayed in the formation, stabilization of ZnO nanoparticles synthesis. The crystal structure and surface morphology were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) and transmittance electron microscopy (TEM) technique.
E-mail address: [email protected] (M. Sundrarajan). http://dx.doi.org/10.1016/j.apt.2015.07.001 0921-8831/Ó 2015 The Society of Powder Technology Japan. Published by Elsevier B.V. and The Society of Powder Technology Japan. All rights reserved.
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The antibacterial activity of the ZnO nanoparticles and ZnO nanoparticles treated cotton fabric were evaluated by agar diffusion method against Escherichia coli and Staphylococcus aureus bacteria.
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2. Materials and methods
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2.1. Materials
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P. pinnata leaves were collected from Karaikudi, Tamil Nadu, India. Zinc nitrate hexahydrate [Zn(NO3)2 6H2O] and citric acid were purchased from Merck, India Pvt. Ltd. Deionised water was used throughout the reaction process.
6% of citric acid as a crosslinking agent. Coating was carried out by pad-dry-cure method [18,19] using the padding mangle at a pressure of 3 psi to get a wet pickup of 100% on weight of fabric. Finally the padded fabric was subjected to air drying and curing at 80 °C and 150 °C for 5 and 3 min respectively.
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2.6. Testing of antibacterial assessment
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The collected leaves were thoroughly washed with water and dried at 30 °C in dust free condition. Dried leaves were crushed into finest powder. 10 g of the powder were boiled with 50 ml of water and extracted under reflux condition at 100 °C for 2 h. After two hours, the aqueous leaves extract were obtained by filtering the mixture through a Whatmann No. 1 filter paper and either directly used in the synthesis of ZnO nanoparticles and stored at 0 °C for further experiments.
The agar diffusion method is a relatively quick and easily effected semi-quantitative test to determine the antibacterial activity [20]. ZnO nanoparticles (100 lg/ml) and treated cotton fabric were tested against S. aureus (gram positive) and E. coli (gram negative) organisms. The suspension of bacteria was grown in nutrient broth medium. Test organisms were dispersed over the surface of agar plates. A small amount of sample is gently pushed over the center of nutrient agar plate inoculated with bacterial cells from intimate contact of the sample. Plates were incubated at 37 °C for 24 h. The antibacterial activity of ZnO nanoparticles and treated cotton fabric were demonstrated by the diameter of the zone of inhibition developed in and around the sample. A zone of inhibition is the area in which the bacterial growth is stopped or prevented due to the bacteriostatic effect of the compound and it measures the inhibitory effect of compound towards a particular microorganism.
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3. Results and discussion
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3.1. XRD analysis
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X-ray diffraction (XRD) analysis was performed on X-ray diffractometer (PANanlytical X-Pert PRO) operated at 40 kV and 30 mA. The pattern was recorded by Cu Ka radiation with about 1.54060 Å. Scanning rate of 2°/min and a sample interval of 0.02° were employed in the 2h range from 20° to 80° for the determination of crystallinity, purity and size of the nanoparticles. The surface morphology of the nanoparticles was examined by JEOL JSM 6390 Scanning electron microscope (SEM) instrument operated at an accelerating voltage at 10 kV. For energy dispersive X-ray (EDX) analysis, the particles were dried on a carbon coated copper grid and performed on SEM instrument equipped with thermo EDX attachment. The FTIR analysis of the zinc oxide nanoparticles was performed by Perkin Elmer make Model Spectrum RX1 (Range 4000 cm 1 –400 cm 1). The UV–Visible spectrum was recorded using JASCO UV–vis. 530 spectrophotometer. TEM images were obtained with a Tecnai 20 G2 (FEI make) Transmission Electron Microscope.
For the first time, ZnO NPs synthesis was carried out using P. pinnata extract via environmentally benign synthetic method. P. pinnata due to their higher constituents of polyphenols are responsible for the formation of ZnO NPs. In this nanoparticles synthesis, aromatic hydroxyl groups present in P. pinnata extract with zinc ions to form the complex with acidic medium [21]. These complexes undergo direct decomposition at 350 °C and leads to formation ZnO NPs. X-ray diffraction pattern is taken in order to confirm phase and crystallinity of the ZnO nanoparticles. The XRD peaks are reliable with the JCPDS data card 89-1397 of hexagonal [22] zinc oxide nanoparticles is displayed in the Fig. 1. The detected peaks corresponded to the hexagonal phase ZnO nanoparticles are found in the lattice planes (h, l, k) of (1 0 0), (0 0 2), (1 0 1), (1 0 2), (1 1 0), (1 0 3), (1 1 2) and (2 0 1) in the 2h value: 31.74°, 34.40°, 36.22°, 47.54°, 56.55°, 62.85°, 67.93° and 69.03° respectively. The
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About 0.1 M zinc nitrate hexahydrate were mixed with 25 ml of extract under vigorous stirring for two hours. After the completion of the reaction, the formed dirty colored precipitate was allowed to settle for 24 h. The precipitate was separated from the reaction solution by centrifugation at 6000 rpm for 15 min, washed with deionised water repeatedly to remove the impurities and dried in an oven at 80 °C. To the powdered as-synthesized sample was then subjected to calcination in muffle furnace at 350 °C for 3 h. TEM sample preparation: 5 lL of ZnO NPs solution was put on a carbon-coated copper grid and was further dried before transferring to the transmission electron microscope.
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2.5. Coating of cotton fabric with ZnO nanoparticles
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Fine medium weight of 100% woven cotton fabric was used for the treatment of biosynthetic ZnO nanoparticles by direct application system. The cotton fabric cut to a size 12 cm 12 cm was immersed in the solution containing 3% of ZnO nanoparticles and
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Intensity (a.u)
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2 Theta Fig. 1. XRD pattern of ZnO nanoparticles.
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Fig. 3. DLS analysis of ZnO nanoparticles.
Fig. 2. UV–Visible spectrum of ZnO nanoparticles.
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crystallite size of the narrow and strong diffraction peak (1 0 1) was 26 nm, determined by Debye–Scherrer’s equation [23]. The narrow peak confirmed the crystallinity of synthesized ZnO nanoparticles.
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3.2. UV–Visible studies
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UV–visible absorption spectroscopy is widely used technique to examine the optical properties of nanosized particles. Fig. 2 shows the peak at 230 nm wavelengths was observed in the UV–visible spectrum, this result confirmed the presence of ZnO nanoparticles synthesized from the leaf extract of P. pinnata which lie much below the band gap wavelength of 358 nm. Thus, there is a strong blue shift in the absorption spectra of the ZnO nanoparticles is indicating that particles must be smaller than the bohr radius of exciton which is for ZnO [24]. This peak is the characteristic of the ZnO formation while confinement in nano scale is proved by blue shift.
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3.3. DLS analysis
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Dynamic light scattering (DLS) is widely being used to measure the size distribution of the prepared ZnO nanoparticles.
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The resulting particle size of ZnO nanoparticles exhibits the size distribution starting from 10 to 120 nm with maximum size distribution is around 90 nm shown in the Fig. 3. Relatively good symmetry of size distribution diagrams in DLS analysis illustrates uniformity of the formed ZnO nanoparticles.
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SEM image is employed to predict the morphology of the ZnO nanoparticles. SEM images of ZnO nanoparticles under different magnifications are displayed in Fig. 4. It is observed that most of the nanoparticles are spherical in shape with agglomeration and confirmed the average size of about 100 nm. The boundary of the single nanoparticles cannot be regarded by intense observation of the SEM images. Further analysis of the ZnO nanoparticles by EDX spectrum in Fig. 5 confirmed the signal characteristic of zinc and oxygen only. All the presented peaks are assigned for Zn and O without any unknown signals proves the purity of ZnO nanoparticles by calcination. The morphology and size of ZnO nanoparticles was confirmed by employing TEM analysis with their corresponding SAED pattern is represented in Fig 6. The TEM image of ZnO nanoparticles are dispersed as a maximum nanorod and hexagonal particles morphology and range in size of 100 nm. Therefore, the nanorod adopts the polycrystalline structure.
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Fig. 4. SEM images of ZnO nanoparticles at different magnification.
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3.5. FT-IR spectroscopy FTIR analysis was performed to determine the functional groups in the synthesis of ZnO NPs. Fig. 7 shows that the FT-IR spectra of ZnO nanoparticles in the 500–4000 cm 1 regions. The broad peak 3403.48 cm 1 was indicate the AOH stretching vibrations. The sharp peak present in the range of 2355.86 cm 1 indicates the free carbonyl group. The peaks at 1714.33 cm 1 is due to the presence of stretching vibrations of C@O bond due to non-ionic carboxylic groups and may be assigned to carboxylic acids or their esters in the natural compound. The band at 1364.80 cm 1 is due to the presence of CAOAH bending mode. It is apparent that the intensity of absorption in the region of 516.52 cm 1 characteristic of hexagonal phase ZnAO vibrations at 350 °C. This suggests that the biological molecules could possibly act as hydrolyzing agent for the metal oxide nanoparticles synthesis.
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3.6. Antibacterial activity of ZnO nanoparticles and treated cotton
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ZnO nanoparticles and treated cotton were tested for its antibacterial activity against the bacterial pathogens, S. aureus (gram positive) and E. coli (gram negative) by agar diffusion method. Zone of inhibition values determined for the treated cotton and ZnO (100 lg/ml) nanoparticles were shown in Table 1. Both treated fabric and ZnO nanoparticles pronounced significant growth inhibitory effect against both bacteria due to their large surface area by their nanosize (Fig. 8). However ZnO nanoparticles treated fabric possess superior antibacterial activity against S. aureus than E. coli bacteria which are clearly visualized in the
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Wavenumber Cm-1 Fig. 7. FT-IR analysis of ZnO nanoparticles.
Table 1 Zone of inhibition (mm) values against test organisms. Samples
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Bacterial Pathogens S. aureus
E. coli
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antibacterial photographs. A gram positive bacterium is thick, cell wall consisting mainly of peptidoglycan surrounding the cytoplasmic membrane and gram negative bacterial cell wall more complex than a gram positive cell, both structurally and chemically. The antibacterial activity may be due to the following assumptions: microorganisms like bacteria have a small pore in cell membrane. Reactive oxygen species (ROS) are generated [25] from the ZnO-nanoparticles actively penetrates the cell membrane using pores of the cell. The leakage of proteins, minerals and some matters from the cell because of the ROS penetrate the cell wall. The cell membrane is damaged, so the bacteria are killed or inhibited of cell growth. Therefore, the present finding clearly revealed that the prepared ZnO nanocrystals using P. pinnata extract could be applied to the fabrics is an excellent antimicrobial activity.
Fig. 6. TEM image of ZnO nanoparticles.
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Fig. 8. Antibacterial activity of (a) ZnO nanoparticles (b) ZnO nanoparticles treated cotton against S. aureus (1) and E. coli (2).
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In this study, a simple, ecofriendly and economic biological process has been developed to synthesize hexagonal phase ZnO nanoparticles via greener method using P. pinnata leaves extract. Crystallization, phase are evaluated by XRD exhibit the crystalline in nature at 350 °C. The ZnO nanoparticles growth limited to about 100 nm is resulted by the DLS, TEM and SEM techniques. Antibacterial activity of ZnO nanoparticles exhibit pronounced skill against the pathogenic bacteria. This types of metal oxide nanoparticles successfully minimize the infections with pathogenic bacteria.
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Acknowledgement
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The authors greatly acknowledge the Department of Physics, Alagappa University for providing XRD (DST-FIST) facilities.
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