Antibacterial Activity of Magnetic Nanoparticles

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characterized by Fourier Transform Infrared (FTIR) spectrometer, X-Ray Diffraction (XRD), and ..... with chemical composition of 98.5% FeCl2 and 1.5% FeCl3.

ISSN 2321 3361 © 2016 IJESC

Research Article

Volume 6 Issue No. 7

Antibacterial Activity of Magnetic Nanoparticles Synthesized from Recycling of Steel Industry Wastes Nagy A.E. Emara1, Souad A. Elfeky2, Rehab M. Amin 3 Assistant Professor 2, 3 Department of Laser Applications in Photochemistry, National Institute of Laser Enhanced Sciences, Cairo University, Giza, 12613, Egypt1, 2, 3 University of Bath, Department of Chemistry, Bath BA2-7AY, UK2 Abstract: Waste acid resulted from the pickling process in steel industries have a high concentration of iron ions that reaches 40 %. The valueless waste acid resulting from steel industries used in the current study for the synthesis of the highly valuable magnetic nanoparticles by co-precipitation method. The surface of the synthesized magnetic nanoparticles was modified by carboxymethylβ-cyclodextrin (CβC) through the copolymerization reactions. The prepared magnetic nanocomposite (CβC/MNCs) was characterized by Fourier Transform Infrared (FTIR) spectrometer, X-Ray Diffraction (XRD), and Transmission Electron Microscope (TEM). The antibacterial activity of the prepared nanocomposite (CβC/MNCs) was evaluated, and results showed a distinct inhibition of both gram-negative and gram-positive strains with various inhibition degrees. Recycling of steel industry waste into valuable magnetic nanoparticles will have a great impact on cleaning up the environment and can be used for microbial disinfection. Keywords: magnetic, nanocomposite, steel industry wastes, recycling, antibacterial Introduction Since the industrial revolution at the beginning of the past century particularly after Bessemer Converter invention iron industry has developed very quickly[1], and the reliance on it becomes the main pillar of any nation progress. The need to increase the mass production increases to cover the continuous demands for steel products, including rebar, railways, vehicles of all kinds, household items and many other uses were, but unfortunately it becomes one of the greatest sources for the disposal of different wastes. The dumps includes heavy smokes emissions during smelting operations, solids wastes including scrap produced by forming stages, and oxides dirties from the end products due to an exposure to the surrounded air, and liquid wastes through preparation processes, such as descaling of iron oxides by using hot acids. To improve steel mechanical characteristics as ductility, hardness, strength, and elongation, iron is alloyed with some elements like carbon, silicon, phosphorus, manganese, chrome, vanadium, ....etc. Consequently the liquid wastes discharge not only contains iron but also contains some of alloyed elements depending on the ratio of their presence in steel caste. During steel processing for platting by zinc alloy or tin alloy additional elements will present in the liquid discharges, where it may contains zinc, lead, nickel, chrome,...etc. During the rolling process for steel, the discharged emulsion may contains many organic compounds in its ingredients so it performs good media for bacterial growth. Drainage of these types of liquid wastes to the industrial and public drainage systems without well treatment could causes serious problems for aquatic and terrestrial environment. One of the new methods to face waste problem is recycling of the waste, so steel scrap melting again or reused by another industries. Liquid wastes usually neutralized according to the traditional methods, then the suspended residues coagulated by using coagulants like ferrous and ferric chlorides, then the accumulated precipitates International Journal of Engineering Science and Computing, July 2016

filtered out by using special type of filters called filter press, the produced sludge can be used in refractory bricks manufacturing, so waste recycling becomes very necessary [2]. One of recycling methods for liquid wastes arises from steel industry, is by generating new valuable materials that can have many environmental desired applications [3]. Particularly, the pickling process using hot hydrochloric acid releases high concentrations of dissolved iron in waste acid. Iron content in can be reached to about 40 % which was found mainly in the form of FeCl2. This dissolved iron can be used as a precursor for the synthesis of magnetic nanoparticles[4],[5]. Materials in nano size characterized by amazing biological characteristics, where as the size deceased to the limit of 1 nm to 100 nm the particles in this case can penetrate easily inside the media that introduced through it; thus it was became possible to use nanoparticles as drug delivery for carrying certain antibiotics to the tumor cells and with the capability for targeting it to the affected cells by the cancer. Also one type of nanoparticle called bucky ball C-60 was used in producing cosmetics creams for treating and fixing the damaged skin layers [6]. In addition to that many types of nano particles have hopeful remarkable resistance for different types of bacteria. For example, nano-silver resist about 650 species of bacteria[7]. Gold nanoparticles surrounded by certain types of antibodies can fluoresce when it hit by particular light wave length and generate sufficient temperature that can easily damaging the targeted cancer cells[8]. As well as nano-iron also have worthy biological activity where it can resist many types of gram-positive and gram-negative bacteria[9]. Also iron and some other nanoparticles were used in field of production and preservation of foods, where it can uses in a safe manner to the human health, so most of the international organizations in field of food and health , and foremost the agency of US Food and Drug Administration (FDA) agree on 8640

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using many types of nano particles for human purposes safely without any recorded side effects [10]. Nanoparticles characteristics can be improved by merging, grafting, coating or capping it with another materials in nano scales, these materials includes natural or synthetic polymers or other metallic nanoparticles which appreciated new characteristics for the two types of nanoparticles, for example iron nanoparticles can coated by gold nano particles giving new useful characteristics in biomedical fields[11], also natural polymers that have long carbon chain as polysaccharides cyclodextrins [12] and chitosan[13] have wide uses in improving characteristics of some nanoparticles when they surrounding it; so nanoparticles will gain new physicochemical properties, high abundance, cheapness, and antimicrobial activity[14], [15]. Although metallic nanoparticles have high surface area, it was considered that it was insufficient, and for increasing it, nanoparticles were surrounded by long chain natural polymers through copolymerization reaction, where this was achieve two desired goals, it increased the active surface area and it give the capability for reusing the polymer after separation for many times.

The separation process in case of iron nanoparticles is more easy where it needs only simple magnet to collect the magnetic nanoparticles which coated with natural polymer or another different nanoparticle, thus it can be used many times in different applications[16],[17]. The aim of the study is to recycle waste hydrochloric acid iron that produced from the pickling process of the steel industry to obtain highly valuable magnetic nonmaterial. This nonmaterial can be modified by copolymerization with natural oligosaccharide carboxymethyl cyclodextrin (β- CD) to become water-soluble and biocompatible nanocomposite. Furthermore, the antimicrobial activity of the prepared nanocomposite against different gram-negative and grampositive strains was tested in this study. Results and Discussion FTIR spectroscopy is the proper technique to understand chemical functionalization of nanoparticles with compounds and polymers. FTIR spectrum in Figure (1) displayed the characteristic peaks for (a) Carboxymethyl- β -Cyclodextrin CβC and (b) the synthesized nanocomposite (CβC/MNCs).

Figure (1): FTIR spectra for (a) Carboxymethyl -β-Cyclodextrin CβC, (b) Unmodified magnetic nanoparticles (FeNPs). and (c) The synthesized nano-composites (CβC/MNCs).

Results showed that, both unmodified magnetic nanoparticles (FeNPs) (Figure 1, b) and The synthesized nano-composites (CβC/MNCs) (Figure 1, c), have the characteristic absorption bands of magnetic part around 568 cm-1 corresponds to Fe-O vibration modes; while the synthesized CβC/MNCs has newly appeared absorption bands at 1065, 1262 and 2936 cm-1 corresponding to –CO,

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C–O–C and C–H bonds in CβC respectively (Figure 1, c). The vibration bands at 2926 and 3400 cm-1 are for C-H and OH groups of CβC respectively. The peaks at 1636 and 1436 cm−1 corresponding to carboxyl (-COO-) groups of CβC (Table 1).

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Table (1): FTIR spectrum frequency (cm-1) for the synthesized unmodified magnetic nanoparticles (FeNPs) and nano-composites (CβC/MNCs). FTIR frequency (cm-1)

Assignment

3650-3250

O–H stretch, carboxylic acids.

2900 - 3000

C-H stretching for carbohydrates

1625

C=O stretching

1550

Asymmetric stretching CO2-

1500

CH2 bending

1350

C -CH3 bending and C- O stretching

1200

C - O - C bending

1125

CH2 bending

915

β- D- glucose

750 - 875 550 - 700

Fe - O - H bending vibrations Fe - O stretching vibration and hematite

500 These bands indicate that CβC moiety has been combined with magnetic nanoparticles successfully, resulting in the formation of the magnetic nanoparticles encapsulated in CβC [18]. X-Ray diffraction patterns ( XRD) used for structural analysis were shown in figure (2), for (a) the prepared unmodified magnetic nanoparticles (FeNPs), and (b) the synthesized nanocomposite (CβC/MNCs). The XRD patterns of FeNPs figure (2a) indicates a highly crystalline cubic structure at diffraction peaks of 30.1, 35.5,43.3, 53.6, 57.0, and 62.6 ° which are corresponding to D220, D311, D400, D422,

Hematite Spheres D511, and D440 respectively for planes of the cubic Fe3O4 lattice. These results are in good agreement with the XRD patterns of MNPs reported in the previous literatures [19],[20],[21],[22], which confirms the cubic spinel structure of the magnetic materials with an average crystal size of 17.02 nm. However it was observed that the XRD patterns of CβC/MNCs figure (2b) have diffractions peaks at 14.09, 27.0, 30.0, 36.4, 43.3, 46.8, 53.0 and 61.6° which are corresponding to D020, D120, D011, D031, D060, D200, D151and D251 respectively for planes of orthorhombic crystal system.

Figure (2): XRD patterns for (a) Unmodified magnetic nanoparticles (FeNPs), and (b) The synthesized nano-composites (CβC/MNCs). The crystallite size of the sample was calculated from peaks using the Debye–Scherrer formula illustrated in the following equation[23]. International Journal of Engineering Science and Computing, July 2016

D=kλ/β cos θ Where k is the Scherrer constant, λ is the X-ray wavelength; β is the peak width of half maximum and θ is the Bragg 8642 http://ijesc.org/

diffraction angle. The calculated average crystal size is 83 nm. The diffraction peaks at 30.1, 35.5, 43.3, 53.6, 57.0, and 62.6 ° of the nanocomposite indicate that the outer shell of CβC/MNCs did not alter the characteristic XRD pattern of magnetic nanoparticles. Also, it stipulated that the superior superparamagnetic properties of iron oxide were maintained after nanocomposite formation. Transmission Electron Microscopy (TEM) is an invaluable tool for the characterization of nanostructures, which can provide the ultimate spatial resolution and analytical sensitivity; where TEM image for the unmodified

magnetic nanoparticles (Figure 3,a) exhibits that the size of nanoparticles are approximately 10-15 nm in diameter and it tends to agglomerate with square like shapes for the cubic crystals. Better dispersion state of the nanocomposites can be observed from the Figure (3, b) with various sizes in diameter from 72 to 102 nm which is comparable to the average size calculated from XRD data (83 nm). The prepared CβC/MNCs display roughly spherical shapes with a core–shell structure consisting of multiple magnetic cores and an outer layer of CβC polymer capsulated around the magnetic nanoparticles

Figure (3): TEM images of (a) unmodified magnetic nanoparticles (FeNPs) and (b) the synthesized nano-composites (CβC/MNCs) . The prepared CβC/MNCs displays roughly spherical shapes negative and gram-positive strains by a micro-well dilution with a core–shell structure consisting of multiple magnetic method using MTT assay. The survival curves of both gramcores and an outer layer of CβC polymer capsulated around negative and gram-positive strains are shown in Figures 4 the magnetic nanoparticles. The synthesized CβC/MNCs and 5. were screened for antibacterial activity against gram-

% of Survival relative to Control

100

S. typhimurium E. coli P. aeruginosa

80

60

40

20

0 0

200

400

600

800

1000

Concentration (g/ml)

Figure (4): Survival curves of Salmonella typhimurium, Escherichia coli and Pseudomonas aeruginosa treated with different concentrations of the synthesized nano-composites (CβC/MNCs). Data points represent mean values ± standard deviation of three independent experiments.

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Analysis of the data of the survival curves of the selected strains of gram-negative bacteria (Figure 4) showed that with increasing concentrations, the survival of Salmonella typhimurium and Escherichia coli decreases in a dosedependent manner whereas up to 90 % & 84 % of bacteria were killed respectively at concentration 1000 µg /ml. In

contrast, results showed that the synthesized CβC/MNCs have no effect on Pseudomonas aeruginosa up to concentration 1000 µg /ml. The antibacterial activity of the synthesized CβC/MNCs towards selected strains of gram-positive bacteria was examined and illustrated in Figure (5).

% of Survival relative to Control

100

B. subtilis S.pneumonia S. aureus

80

60

40

20 0

200

400

600

800

1000

Concentration (g/ml)

Figure (5): Survival curves of Bacillus subtilis, Staphylococcus aureus, and Streptococcus pneumonia treated with different concentrations of the synthesized nano-composites (CβC/MNCs). Data points represent mean values ± standard deviation of three independent experiments. Results showed that the synthesized CβC/MNCs has almost no effect either on Staphylococcus aureus or Streptococcus pneumonia. However, there was a slight decrease in the growth of Streptococcus pneumonia by about 7% starting from concentration 1000 µg /ml. On the other hand, the synthesized CβC/MNCs showed a significant effect on Bacillus subtilis whereas up to 70 % of cells were killed at concentration 1000 µg /ml.

To determine the antagonist potency of the synthesized CβC/MNCs against gram-negative and gram-positive bacteria, MIC50 was calculated and summarized in Table (2) where MIC50 for Salmonella typhimurium, Escherichia coli, and Bacillus subtilis were 108, 215 and 337µg /ml respectively.

Table (2): The Antagonist potency MIC50(µg/ml) for the synthesized nano-composites (CβC/MNCs)against select strains of Gram-negative and Gram-positive bacteria. Organisms

MIC50 (µg/ml) 108 215 337 -

Salmonella typhimurium (RCMB 010077) Escherichia coli (RCMB 010059) Pseudomonas aeruginosa (RCMP 01002 43-5) Bacillus subtilis (RCMB 010067) Staphylococcus aureus (RCMB 010027-8) Streptococcus pneumonia (RCMB 0100199) In general, the synthesized CβC/MNCs had a great antibacterial effect, possibly due to the chelating properties of the magnetic based nanoparticles[24], [25]. These properties may affect the metal transport across the bacterial membranes or bind the bacterial cells at a specific site and thus inhibit their growth. This is in agreement with Huheey

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et al. who mentioned that antibiotics which had chelating properties were able to compete successfully with metalbinding agents of bacteria and thus interfering with their growth[26],[27],[28],[29]. Although the synthesized CβC/MNCs was used at the same concentrations and the number of cells at the beginning of the

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experiment was the same, it is demonstrated that CβC/MNCs showed a higher killing effect on gram negative bacteria than on gram positive bacteria. It was known that gram-negative bacteria have two membranes, the inner and the outer membranes.The inner membrane composed of phospholipids and lipoproteins while the outer one composed mainly of lipopolysaccharide [30]. Therefore, the synthesized CβC/MNCs combine with the lipophilic layer to enhance the membrane permeability of the gram-negative bacteria. The lipid membrane surrounding the cell favors the passage of only lipid-soluble materials; thus, the lipophilicity is an important factor that controls the antimicrobial activity[31]. The cell wall of gram-positive bacteria contains thick polymer layer includes a teichoic acid[32],[33] which gives the outer cell wall negative charge. This negative charge on the cell wall will attract the CβC polymeric part of the synthesized nanocomposites on the surface of the cell wall making disruption in cell signals, thereby hindering the process of protein secretion and slowly penetrate the thick peptidoglycan layer. Conclusion Magnetic-based nanocomposites were successfully prepared from the recycling of Steel Industry wastes with great environmental impact. The surface of the magnetic nanomaterials was functionalized with carboxymethyl-βcyclodextrin (CβC) through the copolymerization reactions. The prepared biocompatible nanocomposite showed a great antibacterial activity against Salmonella typhimurium, Escherichia coli and Bacillus subtilis due to the chelating properties of the magnetic based nanocomposite. Our research is a preliminary step toward developing nanomaterials that could be used for wastewater treatment. As a next step, the chelating properties of the prepared nanocomposites will be examined against heavy metals in wastewater. Experimental 1. Chemicals β -Cyclodextrin (98%) was purchased from WINLAB-U.K. Ammonium hydroxide (25%), Hydrogrn peroxide H2O2(30%) were purchased from LOBA Chemie-India. Sodium hydroxide NaOH (99.9%), Monochloroacetic acid (≥99.0%), and Hydrochloric acid HCl (37%) were purchased from SIGMA-ALDRICH CHEMICAL Co-USA. Epichlorohydrin (≥99.0%), and Iron standard solution 1000 mg/l Fe for AA( iron (III) nitrate nonahydrate in nitric acid 0.5 mol/l) - Scharlau-Spain. Hydrochloric acid as a byproduct of steel Industry waste sample having 34.8 % Iron with chemical composition of 98.5% FeCl 2 and 1.5% FeCl3 was taken from Kandil steel industries, Cairo, Egypt. All chemicals were of the analytical grade and used without additional purification. 2. Synthesis of Carboxymethyl- β -Cyclodextrin (CβC) polymer According to the following steps, CβC polymer was synthesized[34]; 5 g from β – Cyclodextrin (β-CD) was added to 50 ml from 10 % (w/v) NaOH with stirring until they completely mixed. Then 10 ml from Epichlorohydrin was added gradually with intensive stirring for 8 hrs. Another 5 ml from Epichlorohydrin was added with

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continuous stirring for additional three hr. The mixture was lifted overnight at room temperature, then concentrated to 15 ml. Gummy precipitate was grown up after vigorous stirring and washed four times with cold free ethanol. The precipitate was hardened after it washed again with cold acetone; as a result, the high pure yield of βCD/Epichlorohydrin Copolymer of about 80% was obtained. The next essential step in preparing the desired polymer was done by dissolving 4 g from β-CD/Epichlorohydrin Copolymer in 100 ml from 5% (w/v) NaOH solution, then 4 g Monochloroacetic acid was added gradually. The mixture was vigorously stirred for 24 hrs. To neutralizing the excess NaOH, 2M HCl was added drop by drop till pH becomes neutral. The mixture was concentrated to15 ml and cooled over ice to 4ºC. Salt crystals were generated by filtration. The polymer was precipitated by vigorous stirring with cold free ethanol, and washed four times with free ethanol; thus, high pure yield (55%) of CβC was obtained. 3. Preparation of CβC coated magnetic nanocomposite (CβC/MNCs) To prepare the magnetic nanocomposite (CβC/MNCs), 1.5 g from of CβC polymer was dissolved in 40 ml distilled water followed by the addition of 4.77 g from the steel hydrochloric acid waste. Then 15 ml NH4OH (25 % V/V) was mixed gradually with polymer/waste mixture under vigorous stirring (~1200 rpm) for 1 hr at room temperature. 4. Determination of total Iron content and differentiation of its types in waste acid For determining the iron content in waste acid sample two methods were used, the first is instrumentally according to the elemental analysis method by using AA spectrophotometer, this method detects the total iron content without variation between Fe2+ or Fe+3 . Then chemical method was used for determining Fe2+ and Fe+3, the first step for determining Fe2+ or ferrous chloride content, 1.27 g from waste acid was taken, 5 ml of Orthophosphoric acid as media and 55 ml distilled water were mixed together; the mixture titrated with 1M KMnO4 giving the equivalent ferrous volume (V1) ml so Fe% as FeCl2= (V1 x1.27)/Sample weight = a1 %. The second step for determining Fe+3 or ferric chloride content, in 500 ml glass beaker 50 g waste acid was mixed with 50 g concentrated hydrochloric acid (37%), 2 g from zinc powder was added with stirring , after 5 min approximately the reaction completed where the effervescence was stopped. Carefully 0.5 g from this mixture was taken , mixed with 5 ml of Orthophosphoric acid as media and dilute with 55 ml distilled water ; then the mixture titrated with 1M KMnO4 giving the equivalent ferrous volume (V2) ml. Thus Fe% as FeCl2= (V2 x1.27)/Sample weight = a2 %. (a2 %) represents the total iron that found in the total mixture weight (102 g), this method is very sensitive to the weights, so by using the following relation FeCl2 % was detected

a2  Mixture total weight (102 g)

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a1

102

X

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Where X % represents the total iron after reducing all of its types in the sample to be in one form as FeCl2 %., thus X value will be higher than a1%, and the difference between the two ratios represents FeCl3% in the sample.

FeCl3% = X% - a1% The final results showed that the iron content (34.8%) in the used waste acid composed of 98.5% FeCl2, and 1.5% FeCl3. In another way, it can be said the total iron in the waste acid included 34.28% FeCl2 and 0.52% FeCl3. 5. Preparation of Iron nanoparticles (FeNPs) Iron nanoparticles (FeNPs) were prepared from waste acid for comparison study with CβC/MNCs. At the first step, ferrous chloride should partially oxidized to ferric chloride using hydrogen peroxide 3% according to the following chemical equation:

2 FeCl2 + H2O2 + 2 HCl  2 FeCl3 + 2 H2O Where 16.5 g waste acid (which have 34.2% FeCl 2 and 0.5% FeCl3 ) were mixed with 18 ml of H2O2 (3%) solution, with potent stirring for 1h; then gradually 200 ml from NH4OH (25%) solution was added. Reaction temperature was kept at 90Cº, and pH of the solution adapted to be between 8 and 14 for completed precipitation .The solution should left for cooling to room temperature. Black precipitate will come down. The precipitate should washed many times with distilled water until the mixture becomes neutral. The tendency for attraction to simple magnet employed to separate iron nanoparticles easily, then it washed with acetone, and dried in oven at 60-70Cº. 6. Characterization of the prepared CβC/MNCs The infrared spectra (4000.6–399.1 cm−1) were recorded on a Fourier transform infrared spectrometer JASCO FT/IR-4100. X-ray diffraction (XRD) patterns were performed using a PANalytical’s X’Pert PRO diffractometer with Cu Kα radiation. The morphology of the nanocomposite was observed with the transmission electron microscope (FEI Tecnai G2 20 200kV TEM).

50% Dimethyl sulfoxide (DMSO) and then serial of twofold dilutions starting from 3.9 and up to 1000µg/ml were prepared in a 96-well plate. Each well of the microplate included 100 μl of bacterial inoculums and 100 μl of the diluted sample of the prepared composite (CβC/MNCs) whereas, the used inoculums concentration of 5×105CFU/ml was obtained in each well. The plates were then covered with the sterile plate and incubated at 37°C for 24 h. After that, 40 μl of freshly prepared 3- (4, 5-dimethyl-thiazol-2-yl)- 2,5-diphenyltetrazolium bromide (MTT) in water at a final concentration 10mM was added to each well and incubated for 30 min. The change to the red color indicated that the bacteria were biologically active. Color development was measured at λmax 570nm using microplate reader spectroscopy (UV-visible Power wave, Biotech, USA). All experiments were carried out in triplicates. After subtraction of the blank values, the mean values and standard deviations were calculated. Data are presented as percent activity of untreated control. The minimum inhibitory concentrations that cause 50% inhibition of reduction of the dye (MIC50) was calculated from regression curve generated using PRISM (Prism version 4.00 for Windows) non-linear regression analysis for one-phase exponential decay models software (GraphPad Software Inc., San Diego, CA). Acknowledgments This work was sponsored by National Institute of Laser Enhanced Science, Cairo University, Egypt. The authors would like to express the deepest appreciation for Kandil Steel Company, R&D and Chemistry teams there for the help and support. References [1] World Steel Association, The white book of steel. 2012. [2]

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7. Bacteria and Culture Gram-negative bacteria as Salmonella typhimurium (RCMB 010077), Escherichia coli (RCMB 010059), Pseudomonas aeruginosa (RCMP 01002 43-5) and Gram-positive bacteria as Staphylococcus aureus (RCMB 010027-8), Bacillus subtilis (RCMB 010067) and Streptococcus pneumonia (RCMB 0100199) were purchased from the Regional Center for Mycology and Biotechnology- AlAzhar University, Egypt. Bacterial cells were grown for 24 hours on MullerHinton (MH) agar plates at 37°C. The cells were suspended in MH broth media to an optical density (OD) of 0.5 at 595 nm, and diluted with MH broth media to yield a starting inoculums of approximately 106 colony forming units per ml (CFU/ml), which was confirmed by plate counts.

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