Reduce the toxicity of prepared copper sulfide nanoparticles


Department of Applied Science, Biotechnology, University of Technology, Baghdad, Iraq
Department of medical microbiology, College of Medicine, Al-Iraqia University, Baghdad, Iraq

Abstract

Copper sulfide (CuS) nanoparticles have attracted increasing attention from biomedical ‎researchers across the globe, because of their intriguing properties, which have been ‎mainly explored for energy and catalysis related applications. The aim of the study is to ‎prepare CuS NPs by BSA entrapment to reduce the toxicity, characterizing, comparative ‎the toxicity before and after entrapment against bacteria and check the toxicity against RD ‎and L20B cell lines. CuS-BSA NPs was an easy, low toxicity and low cost chemically ‎synthesized. The CuS-BSA NPs was identified though UV-VIS ‎spectrophotometer, FTIR, XRD, SEM, EDX, and Zeta potential. The antibacterial activity ‎against different G-positive and G-negative bacterial strains have been investigated for (2 ‎mg/ml) concentrations of CuS-BSA NPs and commercial CuS. A result showed that CuS-‎BSA NPs have more antibacterial activity than commercial CuS. Using different ‎parameters of CuS-BSA NPs, its anti-cancer bioactivity for every compound synthesized in ‎RD and L20B cell line was explored, and the result proved there was significant toxicity ‎against RD and L20B cell lines.‎

Keywords

Copper sulfide, CuS-BSA, Nanoparticles, Antibacterial, Anticancer, RD cell line, L20B cell line

Introduction

Copper sulfide (CuS) nanoparticles have attracted increasing attention from biomedical ‎researchers around the globe due to their intriguing properties, which have been explored ‎primarily for applications related to energy and catalysis. In vitro, CuS nanoparticles have ‎discovered wide-ranging applications, particularly in the identification of biomolecules, ‎chemicals, pathogens and cancer therapy based on CuS photothermal characteristics, as ‎well as drug delivery and theranostic applications. The progress of CuS nanoparticles has ‎spanned a wide variety of biomedical applications (Goel, Chen, & Cai, 2014).

CuS nanomaterials, in particular, have drawn wide attention due to their low toxicity, ‎simple preparation, low price and high stability (Zhang et al., 2015). On the other side, ‎CuS is commonly used as a material for thermoelectric cooling, optical filers, optical ‎recording equipment, solar cells, nano-scale switches and superionic equipment (Umasankari & Anitha, 2017).

CuS nanoparticles ' ambiguous biotoxicity restricted their biological applications. ‎Developing biocompatible CuS photothermal agents with the capacity for clinical ‎translation is therefore extremely desirable. CuS photothermal nanoparticles using bovine ‎serum albumin (BSA) as a model through mimicking procedures of bio materialization. ‎The toxicity assays in vitro and in vivo showed that BSA-CuS nanoparticles had excellent ‎bio compatibility due to the BSA's intrinsic biocompatibility. Phototherapies were ‎conducted in vitro and in vivo, and excellent outcomes were achieved (Zhang et al., 2015). Furthermore, the results show that the CuS / BSA nanocomposites are ‎approximately one sphere with a size distribution of 10 to 35 nm in diameter and good ‎dispersibility, highly dependent on the concentration of BSA. In biomedical engineering ‎and microelectronics, these protein-assisted synthesized nanocomposites have a huge ‎prospective application. BSA is one of the most commonly researched proteins, and the ‎synthesis of multiple nanocrystals has often been adopted. Preparation methods for CuS / ‎BSA nanocomposites were convenient, easy, non-toxic and environmentally friendly ‎methods for obtaining BSA solution CuS nanoparticles with controllable dimensions and ‎sphere shapes (Huang et al., 2017; M.Y.Radeef, Allawi, & Fawzi, 2018).

The causes of chronic diseases and mortality are bacterial diseases. Because of their ‎cost-effectiveness and strong results, antibiotics were the preferred therapy technique for ‎bacterial diseases. However, several studies have given direct proof that extensive ‎antibiotic use has resulted in multidrug-resistant bacterial strains emerging. In reality, ‎owing to abuse of antibiotics, super-bacteria, which are resistant to almost all antibiotics, ‎have lately evolved. Studies have shown that these bacteria have a gene called NDM-1 ‎with super-resistance. Unfortunately, against each of these modes of action, bacterial ‎resistance may grow. Mechanisms of resistance to current antibiotics have developed ‎from pathogenic bacteria. Developing novel antibacterial therapy techniques that do not ‎relay to traditional therapeutic regimes is urgently needed. Different therapeutic methods ‎for antibiotic-resistant bacteria were created (Wang, Hu, & Shao, 2017).

The consideration of nanoparticles as an alternative to antibiotics is that in some ‎instances, NPs can efficiently prevent resistance to microbial drugs. One of the accepted ‎interactions between nanomaterials and antibacterial activity is that nanomaterials are ‎extremely promising as antibacterial complements to antibiotics and are gaining ‎considerable interest as they could fill the gaps where antibiotics often fail. Moreover, ‎nanomaterials can "as a useful carrier" complement and promote traditional antibiotics (Wang et al., 2017).

It is now well acknowledged that inorganic materials can extinguish bacteria without ‎toxicating the tissue around them. Because of their antibacterial characteristics, copper ‎and its compounds have been used as disinfectants for centuries. CuS nanoparticles ' ‎antimicrobial activities have been studied, suggesting that the activity mainly depends on ‎the morphology of the nanoparticles (Chakraborty, Adhikary, Chatterjee, B.Biswas, & Chattopadhyay, 2016).

Materials and Methods

Chemicals and reagents‎

‎Copper nitrate trihydrate, thioacetamide, bovine serum albumin, copper sulfide and ‎Muller Hinton agar were obtained from Himedia (India). Nitric acid (HNO3) and Dimethyl sulfoxide (DMSO) from BDH (England).3-‎‎(Dimethylthiazol-2-yl) 2,5Diphenyltetrazoliumbromide (MTT) from Sigma (USA). ‎Rhabdomyosarcoma (RD) cell line, as a human cell line, and a murine cell line derived ‎from mouse L cells (L20B) cell line was provided by the Central Public Health Lab., ‎Baghdad, Iraq.

Antibacterial activity‎

Antimicrobial activity of CuS-BSA nanoparticles and CuS commercial separately ‏ ‏were tested against eight bacterial strains (Escherichia coli, Staphylococcus aureus, ‎Staphylococcus epidermis, Salmonella, Klebsiella, Pseudomonas aeruginosa, Proteus, ‎Enterobacter feacalis) by using the agar disk diffusion (Yang, Khan, & Kang, 2015). The test ‎samples were prepared by dissolving CuS-BSA nanoparticles and CuS in distilled water ‎using D.W. solvent as control. Mueller Hinton agar plates were inoculated with active ‎cultured bacteria. Then, a sterile filter paper discs (6 mm in diameter), were loaded with ‎‎20 µl of 2mg/ml concentration of CuS-BSA NPs and CuS commercial then placed on the ‎agar surface. The Plates were incubated at 37 ⁰C for 24 hrs. Antibacterial activity was ‎evaluated by measuring the diameter of the growth inhibition zone against the tested ‎bacteria. ‎

Determination of anticancer activity of CuS-BSA nanoparticles by MTT assay

RD and L20B cell lines were grown in RPMI-1640 medium at 37 °C with 5% CO2 in ‎‎96 – well flat-bottom culture plates at density 1×104 cells /ml for 48 hrs. The cells were ‎treated, in duplicate, with the concentrations of 20 - 70 µg/ml of CuS-BSA NPs and ‎incubated for 24 hrs to determine the toxicity against examined cell lines. 10 µl of MTT ‎solution was added to each well, and the plates were incubated for 4 hrs at 37 ⁰C. The ‎media were then removed, and the remaining formazan crystals were dissolved in DMSO ‎, and the absorbance was measured at 570 nm using an ELISA microplate reader to ‎determine the toxicity of LPS, once with a tumor cell line and another with normal cells. ‎The cytotoxicity percentage was calculated by the equation (Freshney, 2015):

G r o w t h   I n h i b i t i o n   r a t e   %   ( G . I ) = A - B A x   100

A = an optical density of the control. ‎

‎B = an optical density of the treated sample.

Results and Discussion

Characterization‎

UV-VIS spectroscopy analysis

A UV-VIS spectroscopy were used to study the shape and size-controlled nanoparticles in ‎aqueous suspensions. As seen in Figure 1 Absorption spectrum at different wavelengths ‎ranging from 190 to 900 nm were examined to detect the CuS-BSA nanoparticles. The ‎sharp bands of the BSA are observed at 197.5 nm while the spectrum of CuS could be seen ‎at 616 nm. These results were close to a result of (Huang, Li, Hu, & Cui, 2010).

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Figure 1: UV-Vis Spectroscopy scanning of CuS-BSA Nanoparticles

Scanning Electron Microscopic (SEM)

The SEM analysis was conducted to visualize the structure, morphology, and size of ‎CuS-BSA NPs as seen in Figure 2. The SEM CuS-BSA NPs are almost plate-like, and the ‎particle size is in the range of 30–60 nm. This is close to results obtained by (Huang et al., 2010).

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Figure 2: Scanning Electron Microscopic (SEM) image of CuS-BSA

X-Ray Diffraction (XRD) analysis

The XRD pattern of CuS-BSA NPs observed in Figure 3 that show the peaks in the ‎‎2ϴ rang of 5⁰-80⁰. XRD spectrum analysis showed four different strong peaks at 29.1445⁰, ‎‎31.9310⁰, 48.0042⁰ and 59.6812⁰ that are indexed the planes 102, 103, 110 and 203, ‎respectively. According to the Scherrers equation, the larger FWHM values proposed ‎smaller particle size 25 nm and these results agreed with (Chu et al., 2018; Huang et al., 2017; Huang et al., 2010).

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Figure 3: X-ray diffraction analysis of CuS-BSA Nanoparticles

Fourier transform infrared (FTIR) spectroscopy analysis‎

This technique was used to confirm the existence of functional groups in the ‎synthesized CuS-BSA NPs. The FTIR spectra for CuS-BSA NPs were recorded in the ‎spectral region (4000-400) cm−1 as given in Figure 4.‎

The peak at 3435.34 cm-1 is due to the stretching of the N–H bond of amino groups and ‎indicative of bonded hydroxyl (-OH) group. The band at 2928.04 cm-1 is due to alkyl C-H ‎stretching vibration. The band at 2729.37 cm-1 is due to S-H stretching vibration. The ‎FTIR spectrum peak of C=O amide stretch appeared at 1637.62 cm-1. The bands at ‎‎1548.89, 1518.03 cm-1 are attributed to aromatic C=C stretch. The peak at 1386.86 cm−1 is ‎attributed to the absorption of NO3-1, which was introduced by the addition of Cu (NO3)2. ‎The band at 1105.25 cm-1is due to C-O stretching vibration and the band at 1035.81 cm-1 ‎stretching from to C-N stretching of amines. The results were closed to (Chu et al., 2018; Huang et al., 2010; Zhao et al., 2018) when they confirm the existence of ‎functional groups in the synthesized CuS-BSA NPs.‎

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Figure 4: The FTIR spectra for CuS-BSA NPs were recorded in the ‎spectral region

Energy dispersive X-ray spectrum (EDX)

EDX was used to verify the presence of CuS in the suspension of nanoparticles and to ‎determine the chemical composition of CuS-BSA NPs, as shown in Figure 5.

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Figure 5: Energy dispersive X-ray spectrum (EDX); (A) EDX of CuS, (B) Electron image, (C) Table of elements

The results ‎showed the presence of carbon by a large percentage followed by oxygen, nitrogen, copper ‎and sulfur. It should be noted that the element of silicon, magnesium and iron could be ‎attributed to their association with carbon. This result is related to (Chu et al., 2018).

Zeta potential

Zeta potential analysis is important to measure the surface charge of CuS-BSA ‎nanoparticles as demonstrated in Figure 6 the zeta potential value carries a negative ‎charge (-14.49 mV) which means that CuS-BSA NPs solution is stable.‎

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Figure 6: Zeta potential of CuS-BSA Nanoparticles

Antibacterial activity

It was studied ‎against eight bacterial strains; E. coli, S. aureus, S. epidermidis, Salmonella, Klebsiella, ‎Pseudomonas aeruginosa, Proteus, Enterobacter after incubation for 24 hours at 37⁰C. The ‎antibacterial activity of CuS-BSA NPs, at concentration 2 mg/ml, revealed an inhibition ‎zone with a diameter of ‎ ‏)‏ ‎10, 8, 7 and 6‎ ‏(‏ ‎ mm against S. aureus, Proteus, E. coli and Enterobacter respectively, while there is no inhibition zone against Klebsiella, P. ‎aeruginosa, Salmonella and S. epidermidis. The antibacterial activity of commercial CuS, ‎at concentration 2 mg/ml, revealed an inhibition zone with a diameter of 11 and 7 mm ‎against S. epidermidis and S. aureus respectively, while there is no inhibition zone ‎against Klebsiella, P. aeruginosa, Salmonella; E. coli, Proteus and Enterobacter.

The results shown that the antibacterial activity of CuS-BSA NPs against G-ve and G+ve strains, possibly because of the different structures of bacterial walls, as ‎mentioned by (Huang et al., 2017). The antibacterial ‎effects of metallic nanoparticles are greater than other nanomaterials, which demonstrated ‎increasing chemical activity owing to the crystallographic surface structure and their large ‎surface to volume ratios (Wang et al., 2017).

Anticancer

In the current study, the cytotoxic effects of different prepared compounds and ‎complexes against Rhabdomyosarcoma (RD), as human cell line, and murine cell line ‎derived from mouse L cells (L20B) were determined by MTT colorimetric assay. ‎

The cell lines were treated with different concentration of CuS-BSA NPs (20, 30, 40, ‎‎50, 60 and 70 µg/ml) for 24 hours, as shown in Figure 7. The RD cytotoxicity was 58%, ‎at 20 µg/ml that increased gradually to reach 100% when concentrations increased to 70 ‎‎µg/ml, while L20B cells revealed cytotoxicity of 62%, at 20 µg/ml, to reach whole death ‎of cells at a concentration of 70 µg/ml. ‎

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Figure 7: Cytotoxicity of RD and L20B cell lines at different ‎concentrations determined by MTT assay

Conclusion

This study provides an effective way to prepare CuS-BSA NPS nanoparticles from CuS-‎BSA NPs, which is an easy, low-toxic and low-cost way to produce nanoparticles. From ‎this study, CuS-BSA NPs have been found to have a large antibacterial activity with a ‎lower concentration than commercial CuS. ‎

‎The CuS-BSA NPs has proven to have significant toxicity against cancer.‎ The results suggest that CuS-BSA NPs should be further researches for application as drug ‎cancers for other cell lines.‎ In addition, it should be investigated with more different biological activities.‎