Biosynthesis of Nano Nickel Oxide Powder Using Malva sylvestris; Evaluation of Electrocatalytic Activity for Determination of Cephalexin in Real Samples

 Sina Abbasnejad Sina Abbasnejad ,  Banafsheh Norouzi Banafsheh Norouzi
Российский электрохимический журнал
Abstract / Full Text

In the present study, Malva sylvestris leaf extracts was used as a reducing agent for the synthesis of NiO NPs. They were characterized by FT-IR, XRD, and SEM studies. The synthesis of NiO NPs was monitored by different ratios of nickel nitrate solution and extract by using of SEM technique. The average particle size of NiO NPs was 35 nm which is consistent with the particle size calculated by XRD Scherer equation. Also, the carbon paste electrode modified with NiO NPs (NiO NPs/MCPE) was prepared by mixing of NiO NPs and graphite powder. Then, the electrochemical oxidation of cephalexin at the surface of this electrode was investigated using the cyclic voltammetric and amperometric techniques. The presence of NiO NPs markedly enhances the electrocatalytic activity. Under the selected conditions, the anodic peak current was linearly dependent on the concentration of cephalexin in the range of 2.5–35 µM and 65–1.23 × 103 µM by the amperometric method. The detection limit (S/N = 3) was also estimated to be 1.30 µM. This modified electrode was a simple, rapid and effective sensor that was successfully applied to determine cephalexin in the pharmaceutical samples.

Author information
  • Department of chemistry, Qaemshahr Branch, Islamic Azad University, Qaemshahr, Iran

    Sina Abbasnejad &  Banafsheh Norouzi

  1. Yang, H.X., Dong, Q.F., and Hu, X.H., Preparation and characterization of LiNiO2 synthesized from Ni(OH)2 and LiOH·H2O, J. Power Sources, 1999, vol. 79, p. 256.
  2. Miller, E.L. and Rocheleau, R.E., Electrochemical behavior of reactively sputtered iron-doped nickel oxide, J. Electrochem. Soc., 1997, vol. 144, p. 3072.
  3. Hotovy, I., Huran, J., Spiess, L., Capkovic, R., and Hascik, S., Preparation and characterization of NiO thin films for gas sensor applications, Vacuum, 2000, vol. 58, p. 300.
  4. Matsumiya, M., Qiu, F., Shin, W., Lzu, N., Murayama, N., and Kanzaki, S., Thin-film Li-doped NiO for thermoelectric hydrogen gas sensor, Thin Solid Films, 2002, vol. 419, p. 213.
  5. Wang, S.F., Xie, F., and Hu, R.F., Carbon-coated nickel magnetic nanoparticles modified electrodes as a sensor for determination of acetaminophen, Sens Actuators B: Chem., 2007, vol. 123, p. 495.
  6. Ichiyanagi, Y., Wakabayashi, N., Yamazaki, J., Yamada, S., Kimishima, Y., Komatsu, E., and Tajima, H., Magnetic properties of NiO nanoparticles, Phys. B, 2003, vol. 329–333, p. 862.
  7. Makhlouf, S.A., Parker, F.T., Spada, F.E., and Berkowitz, A.E., Magnetic anomalies in NiO nanoparticles, J. Appl. Phys., 1997, vol. 81, p. 5561.
  8. Lok, J.G.S., Geim, A.K., Maan, J.C., Dubonos, S.V., Theil Kuhn, L., and Lindelof, P.E., Memory effects in individual submicrometer ferromagnets, Phys. Rev. B, 1998, vol. 58, p. 12201.
  9. Huang, H., Tian, J., Zhang, W.K., Gan, Y.P., Tao, X.Y., Xia, X.H., and Tu, J.P., Electrochromic properties of porous NiO thin film as a counter electrode for NiO/WO3 complementary electrochromic window, Electrochim. Acta, 2011, vol. 56, p. 4281.
  10. Liu, F., Sang, Y., Ma, H., Li, Z., and Gao, Z., Nickel oxide as an effective catalyst for catalytic combustion of methane, J. Natural Gas Sci. Eng., 2017, vol. 41, p. 1.
  11. Dooley, K.M., Chen, S.Y., and Ross, J.R., Stable nickel-containing catalysts for the oxidative coupling of methane, J. Catal., 1994, vol. 145, p. 402.
  12. Deng, X. and Chen, Z., Preparation of nano-NiO by ammonia precipitation and reaction in solution and competitive balance, Mater. Lett., 2004, vol. 58, p. 276.
  13. Moghaddam, J. and Hashemi, E., Fabrication and characterization of NiO nanoparticles by precipitation from aqueous solution, Korean J. Chem. Eng., 2014, vol. 31, p. 503.
  14. Ghosh, M., Biswas, K., Sundaresan, A., and Rao, C.N.R., MnO and NiO nanoparticles: synthesis and magnetic properties, J. Mater. Chem., 2006, vol. 16, p. 106.
  15. Zhu, Z., Wei, N., Liu, H., and He, Z., Microwave-assisted hydrothermal synthesis of Ni(OH)2 architectures and their in situ thermal convention to NiO, Adv. Powder Technol., 2011, vol. 22, p. 422.
  16. Zhang, X., Shi, W., and Zhu, J., Synthesis of porous NiO nanocrystals with controllable surface area and their application as supercapacitor electrodes, Nano Res., 2010, vol. 3, p. 643.
  17. Nasseri, M.A., Ahrari, F., and Zakerinasab, B., A green biosynthesis of NiO nanoparticles using aqueous extract of Tamarix serotina and their characterization and application, Appl. Organometal. Chem., 2016, vol. 30, p. 978.
  18. Ezhilarasi, A.A., Vijaya, J.J., Kasinathan, K., and Kennedy, L.J., Green synthesis of NiO nanoparticles using Moringa oleifera extract and their biomedical applications: cytotoxicity effect of nanoparticles against HT-29 cancer cells, J. Photochem. Photobiol., 2016, vol. 164, p. 352.
  19. Gilman, A.G., Rall, T.W., Nies, A.S., and Taylor, P., Goodman and Gilman’s the Pharmacological Basis of Therapeutics, New York: Pergamon Press, 1990.
  20. Alwarthan, A.A., Fattah, S.A., and Zahran, N.M., Spectrophotometric determination of cephalexin in dosage forms with imidazole reagent, Talanta, 1992, vol. 39, p. 703.
  21. Murillo, J.A., Rodriguez, J., Lemus, J.M., and Alanon, A., Determination of amoxicillin and cephalexin in mixtures by second-derivative spectrophotometry, Analyst, 1990, vol. 115, p. 1117.
  22. De Paula, C.E.R., Almeida, V.G.K., and Cassella, R.J., Spectrophotometric determination of cephalexin in pharmaceutical formulations exploring its charge transfer reaction with quinalizarin, Quim. Nova, 2010, vol. 33, p. 914.
  23. El-Wasseef, D.R., Spectrofluorometric determination of cephalexin in pharmaceutical preparations and spiked human urine using 2-cyanoacetamide, Spectrosc. Lett., 2007, vol. 40, p. 797.
  24. Yang, J.H., Zhou, G.J., Jie, N.Q., Han, R.J., Lin, C.G., and Hu, J.T., Simultaneous determination of cephalexin and cefadroxil by using the coupling technique of synchronous fluorimetry and H-point standard additions method, Anal. Chim. Acta, 1996, vol. 325, p. 195.
  25. Meng, X. and Peng, J.D., Liquid chromatographic analysis of cephalexin in human plasma by fluorescence detection of the 9-fluorenylmethyl chloroformate derivative, Anal. Lett., 2009, vol. 42, p. 1844.
  26. Oliverira, R.V., De Pietro, A.C., and Cass, Q.B., Quantification of cephalexin as residue levels in bovine milk by high-performance liquid chromatography with on-line sample cleanup, Talanta, 2007, vol. 7, p. 1233.
  27. Steppe, M., Prado, M.S.A., Tavares, M.F.M., Pinto, T.J.A., Kedor-Hackmann, E.R.M., and Santoro, M.I.R.M., Comparison of micellar electrokinetic chromatography, liquid chromatography, and microbiologic assay for analysis of cephalexin in oral suspensions, J. AOAC Int., 2003, vol. 86, p. 707.
  28. Argekar, A.P., Raj, S.V., and Kapadia, S.U., Simultaneous determination of cephalexin and carbocisteine from capsules by reverse phase high performance liquid chromatography (RP-HPLC), Anal. Lett., 1997, vol. 30, p. 821.
  29. Chen, L., Wang, Z., Ferreri, M., Su, J., and Han, B., Cephalexin residue detection in milk and beef by ELISA and colloidal gold based one-step strip assay, J. Agric. Food Chem., 2009, vol. 57, p. 4674.
  30. Zhi, Z.L., Meyer, U.J., van den Bedem, J.W., and Meusel, M., Evaluation of an automated and integrated flow-through immunoanalysis system for the rapid determination of cephalexin in raw milk, Anal. Chim. Acta, 2001, vol. 442, p. 207.
  31. Wei, H., Sun, J.J., Wang, Y.M., Li, X., and Chen, G.N., Rapid hydrolysis and electrochemical detection of trace carbofuran at a disposable heated screen-printed carbon electrode, Analyst, 2008, vol. 133, p. 1619.
  32. Ei-Shaboury, S.R., Salth, G.A., Mohamer, F.A., and Rageh, A.H., Analysis of cephalosporin antibiotics, J. Pharm. Biomed. Anal., 2007, vol. 45, p. 1.
  33. Martinez, LG., Falco, P.C., and Cabeza, A.S., Comparison of several methods used for the determination of cephalosporins, analysis of cephalexin in pharmaceutical samples, J. Pharm. Biomed. Anal., 2002, vol. 2, p. 405.
  34. Farghaly, O.A., Hazzazi, O.A., Rabie, E.M., and Khodari, M., Determination of some cephalosporins by adsorptive stripping voltammetry, Int. J. Electrochem. Sci., 2008, vol. 3, p. 1055.
  35. Li, Q.L. and Chen, S.U., Studies on electrochemical behaviour of cephalexin, Anal. Chim. Acta, 1993, vol. 282, p. 145.
  36. Erceg, M., Kapetanovic, V., Suznjevic, D., and Dumanovic, D., Study of cephalexin and cefaclor adsorption at the mercury/solution interface by AC polarography, Microchem. J., 1997, vol. 57, p. 73.
  37. Devi, A.R., Rani, K.S., and Rao, V.S., Polarographic determination of cephalosporins in pure form and in pharmaceutical preparations, Ind. J. Pharm. Sci., 1994, vol. 56, p. 64.
  38. Norouzi, B. and Mirkazemi, T., Electrochemical sensor for amoxicillin using Cu/poly (o toluidine) (sodium dodecyl sulfate) modified carbon paste electrode, Russ. J. Electrochem., 2016, vol. 52, p. 37.
  39. Norouzi, B., Malekan, A., and Moradian, M., Nickel-zeolite modified carbon paste electrode as electrochemical sensor for hydrogen peroxide, Russ. J. Electrochem., 2016, vol. 52, p. 330.
  40. Norouzi, B. and Norouzi, M., Methanol electrooxidation on novel modified carbon paste electrodes with supported poly(isonicotinic acid) (sodiumdodecyl sulfate)/Ni–Co electrocatalysts, J. Solid State Electrochem., 2012, vol. 16, p. 3003.
  41. Ojani, R., Raoof, J.B., and Norouzi, B., Carbon paste electrode modified by cobalt ions dispersed into poly (N-methylaniline) preparing in the presence of SDS: application in electrocatalytic oxidation of hydrogen peroxide, J. Solid State Electrochem., 2010, vol. 14, p. 621.
  42. Ott, E. and Cairns, R.W., Golden Book of Phase Transitions, Wroclaw, 2002.
  43. Salavati-Niasari, M., Davar, F., Mazaheri, M., and Shaterian, M., Preparation of cobalt nanoparticles from [bis(salicylidene)cobalt(II)]–oleylamine complex by thermal decomposition, J. Magn. Magn. Mater., 2008, vol. 320, p. 575.
  44. Medway, S.L., Lucas, C.A., Kowal, A., Nichols, R.J., and Johnson, D., In situ studies of the oxidation of nickel electrodes in alkaline solution, J. Electroanal. Chem., 2006, vol. 587, p. 172.
  45. Nakamura, M., Tanaka, M., Ito, M., and Sakata, O., Water adsorption on a p (2×2)-Ni(111)–O surface studied by surface X-ray diffraction and infrared reflection absorption spectroscopy at 25 and 140 0K, J. Chem. Phys., 2005, vol. 122, p. 224703. https://doi.org/10.1063/1.1927515
  46. Ojani, R., Raoof, J.B., and Norouzi, B., Performance of glucose electrooxidation on Ni–Co composition dispersed on the poly(isonicotinic acid) (SDS) film, J. Solid State Electrochem., 2011, vol. 15, p. 1139.
  47. Norouzi, B., Sarvinehbaghi, S., and Norouzi, M., Electrocatalytic oxidation of formaldehyde on ni/poly (N,N-dimethylaniline) (sodium dodecylsulfate) modified carbon paste electrode in alkaline medium, Russ. J. Electrochem., 2014, vol. 50, p. 1020.
  48. Bard, A.J. and Faulkner, L.R., Electrochemical Methods, Fundamentals and Applications, New York: John & Wiley, 2001.
  49. Chailapakul, O., Fujishima, A., Tipthara, P., and Siriwongchai, H., Electroanalysis of glutathione and cephalexin using the boron-doped diamond thin-film electrode applied to flow injection analysis, Anal. Sci., 2001, vol. 17, p. 419.
  50. Chen, Y., Huang, L., and Lin, Q., Rapid hydrolysis and electrochemical detection of cephalexin at a heated glassy carbon electrode, Int. J. Electrochem. Sci., 2012, vol. 7, p. 7948.
  51. Xu, M., Ma, H., and Song, J., Polarographic behavior of cephalexin and its determination in pharmaceuticals and human serum, J. Pharm. Biomed. Anal., 2004, vol. 35, p. 1075.
  52. Balooei, M., Raoof, J.B., Chekin, F., and Ojani, R., Cephalexin electrochemical sensors based on glassy carbon modified with 3-mercaptopropyltrimethoxysilane functionalized multi-walled carbon nanotubes, Anal. Bioanal. Electrochem., 2017, vol. 9, p. 929.