GREEN ROUTE SYNTHESIS OF IRON NANOPARTICLES AND ANTIBACTERIAL STUDIES

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1 GREEN ROUTE SYNTHESIS OF IRON NANOPARTICLES AND ANTIBACTERIAL STUDIES 1 NISHIGANDH S. PANDE, 2 DIPIKA KAUR JASPAL, 3 ARTI MALVIYA, 4 JAYACHANDRAN V. P. 1 Symbiosis Institute of Research and Innovation (SIRI), A Constituent of Symbiosis International University (SIU), Symbiosis Institute of Technology (SIT), Lavale, Pune , Maharashtra State, India 2 Symbiosis Institute of Technology (SIT), Symbiosis International University (SIU), Gram: Lavale, Tal. Mulshi, Pune , Maharashtra INDIA 3 Lakshmi Narain College of Technology, Bhopal , Madhya Pradesh, INDIA 4 Antibacterials and Microbial Technology Lab, Pushpagiri Research Centre, Pushpagiri Institute of Medical Sciences, Tiruvall , INDIA Abstract- Eco-friendly synthesis of iron nanoparticles was achieved by a novel, facile green route method using Abelmoschus esculentus as a reducing and capping agent. The successful formation of iron nanoparticles has been confirmed by X-ray diffraction, UV-visible, FTIR, FE-SEM and TEM analysis. The prepared nanoparticles have been tested for antibacterial activity for Escherichia Coli (Gram negative) and Staphylococcus aureus (Gram positive). Keywords - Antibacterial Study, Ecofriendly Synthesis, Iron Nanoparticles, Natural Binder. I. INTRODUCTION Nanoscience is an upcoming topic of interest in the field of materials chemistry. Optimization of the synthesis parameters to obtain nanomaterials in the size range of nm and the investigation of properties is the area covered under nanoscience. Nanoscale materials show size dependent properties different from the corresponding bulk or molecule. Recent researches have been focused towards the synthesis of these nanoparticles by eco-friendly methods. Nanocrystalline iron particles, a topic of interest in the present research, have found various applications in several research areas such as biomedicine[1], catalyst [2], batteries [3], sensor [4], bimolecular detection [5] etc. In the last few years, various synthesis techniques have been developed to produce iron nanoparticles such as electrochemical synthesis [6], laser pyrolysis technique [7], chemical reduction [8] etc. The main concentration nowadays is to develop economical and environmentally clean synthesis methods to synthesize iron nanoparticles. Numerous ecofriendly materials have been used for synthesis of iron nanoparticles like plant extracts [9] etc. for the same. These eco friendly techniques do not require high temperature, pressure or the use of toxic chemicals. In the present research paper, such an ecofriendy synthesis method for iron nano particles has been reported using the solutions of FeCl 3 and FeSO 4 by the aqueous extract of a natural material Abelmoschus esculentus. The nanoparticles synthesized by the mentioned ecofriendly method were found toxic for bacteria like Escherichia Coli (Gram negative) and Staphylococcus aureus (Gram positive). II. METHOD OF ANALYSIS Materials FeCl 3, FeSO 4, used for the synthesis were analytical grade (Aldrich chemical). All the aqueous solutions were prepared with deionized water. Synthesis of Iron nanoparticles Solution of 0.05 M FeSO 4 and M FeCl 3 solution were prepared in deionized water. 70 ml of the vegetable extract of Abelmoschus esculentus (Okra) was mixed with 10 ml of 0.05 M FeSO 4 and M FeCl 3 solution in the sonocator at a temperature of 60 C. The formation of yellow to dark green colour was observed indicating the formation of nanoparticles. Antibacterial study Weighed amount of HIMEDIA was dissolved in 500 ml of distilled water. The ph of the medium was adjusted to 7.4 by using 1N NaOH. The medium was heated to dissolve agar and to form a clear liquid. Distilled water was added to make final volume. It was sterilized in autoclave at 121 C, 15 lb pressure for 15 minutes. The flask was allowed to cool up to 50 C and then the medium was quickly poured into sterile plates under aseptic conditions. The medium was allowed to cool so as to produce solid agar plates. The plates were inoculated by specific microorganism by spread plate technique and allowed to dry; wells were made in the solidified agar plate by using a sterile borer. Test solution of specified concentration was then added in the well by using sterile pipette and the plates were then kept in freeze for 1hour for diffusion followed by incubation at 37 C for 24 hours. 74

2 III. RESULTS AND DISCUSSIONS UV-visible spectra The UV-vis spectra of iron nanoparticles synthesized by Abelmoschus esculentus (okra) extract is shown in figure 1. An absorption peak observed at 415 nm[10]-[11]. After the addition of Ferrous sulphate (FeSO 4 ) and Ferric chloride (FeCl 3 ) solution, the colour of the solution changes from faint yellow to green indicating the synthesis of iron nanoparticles in the aqueous medium[12]. Green Route Synthesis of Iron Nanoparticles and Antibacterial Studies Fig. 2 FTIR absorption spectra of Iron nanoparticles binded with Abelmoschus Esculentus (okra) extract. X-ray diffraction The formation of iron nanoparticles using Abelmoschus esculentus extract was further confirmed by X-ray diffraction (XRD) analysis. The observed peak at (2 ) was attributed to the 113 plane, which exhibited good crystallinity. A broad peak indicated the size in nano scale, which matches with standard JCPDS number [16]-[17]. The particles size was determined using Scherrer s formula, D= 0.9λ/βcosθ was estimated at 24 Fig. 1 UV-visible spectra of Iron nanoparticles Fourier transform infrared spectroscopy (FTIR) FTIR measurements of Ag-nanoparticles with Abelmoschus esculentus (Okra) showed the presence of bands at 582, 982, 1041, 1122, 1200, 1367, 1565,1769, 2902, 3259 and 3510 cm -1 (figure 2). The bands at 1565 and 1367 cm -1 corresponded to C-C and C-N stretching respectively indicating the presence of ligands similar to those found in biopolymers (proteins, carbohydrates) [13]. The region of cm -1 showed band is corresponding to OH stretching vibration. C-H stretching vibration due to the presence of CH and CH 2 was observed at 2902 cm -1. C=O stretching vibration was well represented at 1769 cm -1. Anti-symmetrical deformation of C-O-C resulted in a peak at 1122 cm -1 [14]. Fe-O bond observed at 582 cm -1 [15]. Fig. 3 X-ray diffractogram of Iron nanoparticles synthesized from Abelmoschus esculentus (okra) extract. Field emission scanning electron microscopy (FE-SEM) FE-SEM analysis results of iron nanoparticles were clearly distinguishable at different enlargements. Iron nanoprticles in the Abelmoschus esculentus extract ( natural polymer) were found to be polydispersed ( figure 5 ) and measured in size from 24 to 34 75

Green Route Synthesis of Iron Nanoparticles and Antibacterial Studies Fig.

7 TEM image of spherical shaped Iron nanoparticles at 200 Fig.

electron microscopy (TEM) Iron nanoparticles size was found between 20 to 34 nm,

$The selected area electron diffraction pattern (SAED) studies showed the$ 17 Å, in good agreement with the planes (113), for spherical iron nanoparticles

17 Å, in good agreement with the planes (113), for spherical iron nanoparticles

8 TEM image of spherical shaped Iron nanoparticles at 100 Fig.

3 Green Route Synthesis of Iron Nanoparticles and Antibacterial Studies Fig. 4 FE-SEM image of spherical shaped Iron nanoparticles at 1 µm Fig. 7 TEM image of spherical shaped Iron nanoparticles at 200 Fig. 5 FE-SEM image of spherical shaped Iron nanoparticles at 500 Transmission electron microscopy (TEM) Iron nanoparticles size was found between 20 to 34 nm, which nearly matched with the TEM (figures 6-10) as well as XRD results. The selected area electron diffraction pattern (SAED) studies showed the nanocrystalline nature and corresponded to the interplanar distances of 1.17 Å, in good agreement with the planes (113), for spherical iron nanoparticles (figure 11)[18]-[21]. Fig. 8 TEM image of spherical shaped Iron nanoparticles at 100 Fig. 6 TEM image of spherical shaped Iron nanoparticles at 500 Fig. 9 TEM image of spherical shaped Iron nanoparticles at 50 Proceedings of 20th IRF International Conference, 22nd February 2015, Pune, India, ISBN:

Green Route Synthesis of Iron Nanoparticles and Antibacterial Studies V. COMPARISON OF RESULTS Iron nanoparticles showed antibacterial activity against pathogenic E. coli and S.

aureus, here in proved antibacterial activity gave positive results at low concentration [22]-[23]. CONCLUSIONS Fig.

4 Green Route Synthesis of Iron Nanoparticles and Antibacterial Studies V. COMPARISON OF RESULTS Iron nanoparticles showed antibacterial activity against pathogenic E. coli and S. aureus at concentration around 9 mg/ml and 3 mg/ml respectively. Based on previously reported results of E. coli and S. aureus, here in proved antibacterial activity gave positive results at low concentration [22]-[23]. CONCLUSIONS Fig. 10 TEM image of spherical shaped Iron nanoparticles at 20 (113) Iron nanoparticles were synthesized successfully by using Abelmoschus esculentus (natural polymer). The Iron nanoparticles were spherical as confirmed by TEM technique. The size of iron nanoparticles ranged from 24 to 34 Iron nanoparticles showed good antibacterial activity against E.coli and S.aureus. ACKNOWLEDGEMENT One of the authors (NP) is thankful to CMET, Pune for providing instrumentation for characterization of FE-SEM and TEM micrographs. The help provided by ISSER, Pune is also greatly acknowledged for the support in recording XRD, FTIR, UV-Visible spectra of the prepared sample. REFERENCES Fig. 11 SAED of iron nanoparticles. IV. ANTIBACTERIAL ACTIVITY The iron nanoparticles showed antibacterial activity against strain of gram negative and gram positive bacteria, which was effective against Escherichia Coli and Staphylococcus aureus respectively. The plates were examined after 24 hours of incubation and zone of inhibition was measured at 37 C. Iron nanoparticles solution with concentrations 500 µg/ml and 250 µg/ml were added for investigating the activity of Escherichia Coli and Staphylococcus aureus respectively, using a micropipette. The diameter of the zone to the nearest millimeter across the well was recorded. The results obtained after 24 hours has shown in table 1. Table. 1 Zone of inhibition of S.aureus and E.coli [1] C.C. Berry, A. S. Curtis, "Functionalisation of magnetic nanoparticles for applications in biomedicine," Journal of physics D: Applied physics, vol. 36, no.13, pp , June [2] J.M. Yan, X.B. Zhang, S. Han, H. Shioyama, Q. Xu, "Iron Nanoparticle Catalyzed Hydrolytic Dehydrogenation of Ammonia Borane for Chemical Hydrogen Storage," Angewandte Chemie International Edition, vol.47, no.12, pp ,Feb [3] B.Koo, H. Bonil, Koo, B., H. Xiong, M. D. Slater, V. B. Prakapenka, M. Balasubramanian, P. Podsiadlo, E. V. Shevchenko,"Hollow iron oxide nanoparticles for application in lithium ion batteries," Nano letters, vol. 12, no.5,pp , April [4] B. Fang, G. Wang, W. Zhang, M. Li, X. Kan,"Fabrication of Fe 3O 4 nanoparticles modified electrode and its application for voltammetric sensing of dopamine," Electroanalysis, vol.17, no.9, pp , April [5] D. J. Maxwell, J. R. Taylor, S. Nie, "Self-assembled nanoparticle probes for recognition and detection of biomolecules," Journal of the American Chemical Society, vol.124, no.32, pp , July [6] C. Pascal, J. L. Pascal, F. Favier, M. L. Elidrissi Moubtassim, C. Payen, "Electrochemical synthesis for the control of γ-fe 2O 3 nanoparticle size. Morphology, microstructure, and magnetic behavior,"chemistry of materials, vol.11, no.1, pp , Dec [7] O. Bomatí-Miguel, L. Mazeina, A. Navrotsky, S. Veintemillas-Verdaguer, "Calorimetric study of maghemite 77

5 Green Route Synthesis of Iron Nanoparticles and Antibacterial Studies nanoparticles synthesized by laser-induced pyrolysis," Chemistry of Materials, vol. 20, no.2, pp , Jan [8] K. C. Huang, S. H. Ehrman, "Synthesis of iron nanoparticles via chemical reduction with palladium ion seeds," Langmuir, vol.23, no.3, pp , Dec [9] M. Pattanayak, P. L. Nayak, Ecofriendly Green Synthesis of Iron Nanoparticles From Various Plants And Spices Extract, International Journal of Plant, Animal and Environmental Sciences, vol. 3, no.1, pp , Dec [10] M. Mazur, A. Barras, V. Kuncser, A. Galatanu, V. Zaitzev, K. V. Turcheniuk, S. Szunerits, "Iron oxide magnetic nanoparticles with versatile surface functions based on dopamine anchors," Nanoscale, vol.5, no.7, pp , Jan [11] M. Mahdavi, F. Namvar, M. B. Ahmad, R. Mohamad, Green biosynthesis and characterization of magnetic iron oxide (Fe 3O 4) nanoparticles using seaweed (Sargassum muticum) aqueous extract, Molecules, vol.18, no.5, pp , May [12] S. K. Kulkarni, Nanotechnology: Principles and Practices, Capital Publishing Company, ISBN , pp , [13] J. Cookson, "The preparation of palladium nanoparticles," Platinum Metals Review, vol.56, no.2, pp , April [14] I. M. De Rosa, J. M. Kenny, D. Puglia, C. Santulli, F. Sarasini, "Morphological, thermal and mechanical characterization of okra (Abelmoschus esculentus) fibres as potential reinforcement in polymer composites." Composites Science and Technology, vol.70, no.1, pp , Sept [15] R. Palanivel, G. Velraj, "FTIR and FT-Raman spectroscopic studies of fired clay artifacts recently excavated in Tamilnadu, India," Indian journal of pure and applied physics, vol. 45, no.6, pp , Jun [16] S. Laurent, D. Forge, M. Port, A. Roch, C. Robic, L. Elst Vander, R. N. Muller, Magnetic Iron oxide nanoparticles: synthesis, stabilization, verctorization, physicochemical characterization and biological application, Chemical reviews, vol. 108, no.6, pp , April [17] M. Mikhayloya, D. K. Kim, C. C. Berry, A. Zagorodni, M. Toprak, A. S. Curtis, M. Muhammed, BSA immobilization on amine-fuctionalized superparameagnetic iron oxide nanoparticles, Chemical of materials, vol.16, no.12, pp , May [18] S. J. Park, S. Kim, S. Lee, Z. G. Khim, K. Char, T. Hyeon, Synthesis and magnetic studies of uniform iron nanorods and nanoshperes, Journal of the Americal Chemical Society, Vol.122, no.35, pp , May [19] N. Aguiló-Aguayo, M. J. Inestrosa-Izuieta, J. Garcia-Cespedes, E. Bertran, "Morphological and magnetic properties of superparamagnetic carbon-coated Fe nanoparticles produced by arc discharge," Journal of nanoscience and nanotechnology, vol. 10, no.4, pp , April [20] B. Kumar, K. Smita, L. Cumbal, A.Debut, "Biogenic synthesis of iron oxide nanoparticles for 2-arylbenzimidazole fabrication," Journal of Saudi Chemical Society, vol.18, no.4, pp , Sept [21] S. Bagheri, K. G. Chandrappa, S. B. A. Hamid, Generation of Hematite Nanoparticles via Sol-Gel Method, Research Journal of Chemical Sciences, vol.3, no. 7, pp.62-68, July [22] N. Tran, A. Mir, D. Mallik, A. Sinha, S. Nayar, T. J. Webster,"Bactericidal effect of iron oxide nanoparticles on Staphylococcus aureus," International journal of nanomedicine, vol. 5, pp , April [23] C. Lee, J. Y. Kim, W. I. Lee, K. L. Nelson, J. Yoon, D. L. Sedlak, "Bactericidal effect of zero-valent iron nanoparticles on Escherichia coli," Environmental science & technology, vol. 42, no.13, pp , May

FACILE GREEN ROUTE SYNTHESIS OF SILVER NANOPARTICLES USING NATURAL POLYMER AND THEIR ANTIBACTERIAL ACTIVITY

CELLULOSE CHEMISTRY AND TECHNOLOGY FACILE GREEN ROUTE SYNTHESIS OF SILVER NANOPARTICLES USING NATURAL POLYMER AND THEIR ANTIBACTERIAL ACTIVITY NISHIGANDH S. PANDE, DIPIKA KAUR JASPAL, * ANIRUDHA CHABUKSWAR,