Applied Nanoscience

, Volume 9, Issue 3, pp 371–385 | Cite as

The effect of phenolic compounds on the green synthesis of iron nanoparticles (FexOy-NPs) with photocatalytic activity

  • Pablo Salgado
  • Katherine Márquez
  • Olga Rubilar
  • David Contreras
  • Gladys VidalEmail author
Original Article


The green synthesis of nanoparticles allows for obtaining nanomaterials using plant extracts, avoiding the use of toxic and dangerous chemical compounds. The aim of this study was to evaluate the effect of phenolic compounds in plant extracts on the synthesis of iron oxide nanoparticles (FexOy-NPs) with photocatalytic activity. Accordingly, the phenolic content in 11 plant extracts was evaluated by the Folin–Ciocalteu (F–C) method, and the iron-reducing capacity was evaluated by the ferric-reducing antioxidant power method (FRAP). From the F–C and FRAP analyses, the Luma apiculata (LAL), Phragmites australis (PAL) and Eucalyptus globulus (EGL) extracts were selected and analyzed by HPLC coupled with a diode array detector (DAD) to identify and quantify the phenolic compounds. Using the three selected extracts, FexOy-NPs were synthesized, which were then characterized by UV–Vis spectroscopy, FTIR, DLS, zeta potential, SEM-EDX, and Raman and diffuse reflectance spectroscopy. The SEM-EDX, DLS and zeta potential analyses showed that the FexOy-NPs were spherical, stable and nanosized. The FRAP, F–C and FTIR analyses indicated the role of phenolic compounds in the formation and stabilization of FexOy-NPs. It was possible to establish a direct relationship between the composition of the phenolic compounds and the reducing capacity of the extracts. In addition, it was found that phenolic compounds and their concentrations are associated with the size and type of FexOy-NPs obtained. Furthermore, it was proposed that types of phenolic compounds influence the formation of different phases of FexOy-NPs. The photocatalytic activity of the FexOy-NPs was demonstrated by diffuse reflectance spectroscopy and decolorization of a dye under visible radiation.


Luma apiculata Phragmites australis Eucalyptus globulus Leaf extracts Dye decolorization 



This research was supported by CONICYT/FONDAP/15130015. Pablo Salgado would like to thank Project CONICYT FONDECYT/Postdoctorado 3180566. The authors would like to thank the Centro de Microscopía Avanzada, CMA BIO–BIO Proyecto CONICYT PIA ECM-12; Interdisciplinary Group of Advanced Nanocomposites of the School of Engineering, University of Concepción and its Project CONICYT FONDEQUIP/EQM 150139; Project CONICYT FONDEQUIP/EQM 140088; and the Laboratory of Organic Environmental Chemistry for its spectroscope of diffuse reflectance.


  1. Almeida I, Fernandes E, Lima J, Valentão P, Andrade P, Seabra R, Costa P, Bahia M (2009) Oxygen and nitrogen reactive species are effectively scavenged by eucalyptus globulus leaf water extract. J Med Food 12:175–183. CrossRefGoogle Scholar
  2. Anouar EH, Gierschner J, Duroux J-L, Trouillas P (2012) UV/Visible spectra of natural polyphenols: a time-dependent density functional theory study. Food Chem 131:79–89. CrossRefGoogle Scholar
  3. Berker KI, Guclu K, Demirata B, Apak R (2010) A novel antioxidant assay of ferric reducing capacity measurement using ferrozine as the colour forming complexation reagent. Anal Methods 2:1770–1778. CrossRefGoogle Scholar
  4. Bersani D, Lottici P, Montenero A (1999) Micro-Raman investigation of iron oxide films and powders produced by sol–gel syntheses. J Raman Spectrosc 30:355–360.;2-C CrossRefGoogle Scholar
  5. Bishnoi S, Kumar A, Selvaraj R (2018) Facile synthesis of magnetic iron oxide nanoparticles using inedible Cynometra ramiflora fruit extract waste and their photocatalytic degradation of methylene blue dye. Mater Res Bull 97:121–127. CrossRefGoogle Scholar
  6. Burgos V, Araya F, Reyes-Contreras C, Vera I, Vidal G (2017) Performance of ornamental plants in mesocosm subsurface constructed wetlands under different organic sewage loading. Ecol Eng 99:246–255. CrossRefGoogle Scholar
  7. Calheiros CSC, Bessa VS, Mesquita RBR, Brix H, Rangel AOSS, Castro PML (2015) Constructed wetland with a polyculture of ornamental plants for wastewater treatment at a rural tourism facility. Ecol Eng 79:1–7. CrossRefGoogle Scholar
  8. Castillo RdP, Araya J, Troncoso E, Vinet S, Freer J (2015) Fourier transform infrared imaging and microscopy studies of Pinus radiata pulps regarding the simultaneous saccharification and fermentation process. Anal Chim Acta 866:10–20. CrossRefGoogle Scholar
  9. Cornell RM, Schwertmann U (2003) The iron oxides: structure, properties, reactions, occurrences and uses. Wiley, New YorkCrossRefGoogle Scholar
  10. Davis EA, Mott NF (1970) Conduction in non-crystalline systems V. Conductivity, optical absorption and photoconductivity in amorphous semiconductors. Philos Mag 22:0903–0922. CrossRefGoogle Scholar
  11. Devatha CP, Thalla AK, Katte SY (2016) Green synthesis of iron nanoparticles using different leaf extracts for treatment of domestic waste water. J Clean Prod 139:1425–1435. CrossRefGoogle Scholar
  12. Durán N, Cuevas R, Cordi L, Rubilar O, Diez MC (2014) Biogenic silver nanoparticles associated with silver chloride nanoparticles (Ag@AgCl) produced by laccase from Trametes versicolor. SpringerPlus 3:645. CrossRefGoogle Scholar
  13. El-Moslamy SH, Elkady MF, Rezk AH, Abdel-Fattah YR (2017) Applying Taguchi design and large-scale strategy for mycosynthesis of nano-silver from endophytic Trichoderma harzianum SYA.F4 and its application against phytopathogens. Sci Rep 7:45297. CrossRefGoogle Scholar
  14. Fazlzadeh M, Rahmani K, Zarei A, Abdoallahzadeh H, Nasiri F, Khosravi R (2017) A novel green synthesis of zero valent iron nanoparticles (NZVI) using three plant extracts and their efficient application for removal of Cr(VI) from aqueous solutions. Adv Powder Technol 28:122–130. CrossRefGoogle Scholar
  15. Fuentes N, Pauchard A, Sánchez P, Esquivel J, Marticorena A (2013) A new comprehensive database of alien plant species in Chile based on herbarium records. Biol Invasions 15:847–858. CrossRefGoogle Scholar
  16. Iravani S (2011) Green synthesis of metal nanoparticles using plants. Green Chem 13:2638–2650. CrossRefGoogle Scholar
  17. Kähkönen MP, Hopia AI, Vuorela HJ, Rauha J-P, Pihlaja K, Kujala TS, Heinonen M (1999) Antioxidant activity of plant extracts containing phenolic compounds. J Agric Food Chem 47:3954–3962. CrossRefGoogle Scholar
  18. Lin J, Weng X, Dharmarajan R, Chen Z (2017) Characterization and reactivity of iron based nanoparticles synthesized by tea extracts under various atmospheres. Chemosphere 169:413–417. CrossRefGoogle Scholar
  19. Lu W, Shen Y, Xie A, Zhang W (2010) Green synthesis and characterization of superparamagnetic Fe3O4 nanoparticles. J Magn Magn Mater 322:1828–1833. CrossRefGoogle Scholar
  20. Machado S, Pinto SL, Grosso JP, Nouws HPA, Albergaria JT, Delerue-Matos C (2013) Green production of zero-valent iron nanoparticles using tree leaf extracts. Sci Total Environ 445–446:1–8. CrossRefGoogle Scholar
  21. Martínez-Cabanas M, López-García M, Barriada JL, Herrero R, Sastre de Vicente ME (2016) Green synthesis of iron oxide nanoparticles. Development of magnetic hybrid materials for efficient As(V) removal. Chem Eng J 301:83–91. CrossRefGoogle Scholar
  22. Mondal P, Purkait MK (2018) Green synthesized iron nanoparticles supported on pH responsive polymeric membrane for nitrobenzene reduction and fluoride rejection study: Optimization approach. J Clean Prod 170:1111–1123. CrossRefGoogle Scholar
  23. Nidheesh PV, Gandhimathi R, Velmathi S, Sanjini NS (2014) Magnetite as a heterogeneous electro Fenton catalyst for the removal of Rhodamine B from aqueous solution. RSC Adv 4:5698–5708. CrossRefGoogle Scholar
  24. Nieuwoudt MK, Comins JD, Cukrowski I (2011) The growth of the passive film on iron in 0.05 M NaOH studied in situ by Raman micro-spectroscopy and electrochemical polarisation. Part I: near-resonance enhancement of the Raman spectra of iron oxide and oxyhydroxide compounds. J Raman Spectrosc 42:1335–1339. CrossRefGoogle Scholar
  25. Pang YL, Lim S, Ong HC, Chong WT (2016) Research progress on iron oxide-based magnetic materials: synthesis techniques and photocatalytic applications. Ceram Int 42:9–34. CrossRefGoogle Scholar
  26. Perron NR, Brumaghim JL (2009) A review of the antioxidant mechanisms of polyphenol compounds related to iron binding. Cell Biochem Biophys 53:75–100. CrossRefGoogle Scholar
  27. Prior RL, Wu X, Schaich K (2005) Standardized methods for the determination of antioxidant capacity and phenolics in foods and dietary supplements. J Agric Food Chem 53:4290–4302. CrossRefGoogle Scholar
  28. Rabbani M, Rafiee F, Ghafuri H, Rahimi R (2016) Synthesis of Fe3O4 nonoparticles via a fast and facile mechanochemicl method: modification of surface with porphyrin and photocatalytic study. Mater Lett 166:247–250. CrossRefGoogle Scholar
  29. Rengasamy M, Anbalagan K, Kodhaiyolii S, Pugalenthi V (2016) Castor leaf mediated synthesis of iron nanoparticles for evaluating catalytic effects in transesterification of castor oil. RSC Adv 6:9261–9269. CrossRefGoogle Scholar
  30. Salgado P, Melin V, Contreras D, Moreno Y, Mansilla HD (2013) Fenton reaction driven by iron ligands. J Chil Chem Soc 58:2096–2101. CrossRefGoogle Scholar
  31. Sarkar J, Mollick MMR, Chattopadhyay D, Acharya K (2017) An eco-friendly route of γ-Fe2O3 nanoparticles formation and investigation of the mechanical properties of the HPMC-γ-Fe2O3 nanocomposites. Bioproc Biosyst Eng 40:351–359. CrossRefGoogle Scholar
  32. Sepúlveda-Mardones M, López D, Vidal G (2017) Methanogenic activity in the biomass from horizontal subsurface flow constructed wetlands treating domestic wastewater. Ecol Eng 105:66–77. CrossRefGoogle Scholar
  33. Shahwan T, Abu Sirriah S, Nairat M, Boyacı E, Eroğlu AE, Scott TB, Hallam KR (2011) Green synthesis of iron nanoparticles and their application as a Fenton-like catalyst for the degradation of aqueous cationic and anionic dyes. Chem Eng J 172:258–266. CrossRefGoogle Scholar
  34. Shamaila S, Sajjad AKL, Ryma N-u-A, Farooqi SA, Jabeen N, Majeed S, Farooq I (2016) Advancements in nanoparticle fabrication by hazard free eco-friendly green routes. Appl Mater Today 5:150–199. CrossRefGoogle Scholar
  35. Sharma P, Kumar R, Chauhan S, Singh D, Chauhan M (2014) Facile growth and characterization of α-Fe2O3 nanoparticles for photocatalytic degradation of methyl orange. J Nanosci Nanotechno 14:6153–6157. CrossRefGoogle Scholar
  36. Sherman DM (2005) Electronic structures of iron(III) and manganese(IV) (hydr)oxide minerals: thermodynamics of photochemical reductive dissolution in aquatic environments. Geochim Cosmochim Acta 69:3249–3255. CrossRefGoogle Scholar
  37. Shi A, Chen X, Liu L, Hu H, Liu H, Wang Q, Agyei D (2017) Synthesis and characterization of calcium-induced peanut protein isolate nanoparticles. RSC Adv 7:53247–53254. CrossRefGoogle Scholar
  38. Simirgiotis MJ, Bórquez J, Schmeda-Hirschmann G (2013) Antioxidant capacity, polyphenolic content and tandem HPLC–DAD–ESI/MS profiling of phenolic compounds from the South American berries Luma apiculata and L. chequén. Food Chem 139:289–299. CrossRefGoogle Scholar
  39. Szymczycha-Madeja A, Welna M, Zyrnicki W (2013) Multi-element analysis, bioavailability and fractionation of herbal tea products. J Brazil Chem Soc 24:777–787. Google Scholar
  40. Tauc J, Grigorovici R, Vancu A (1966) Optical properties and electronic structure of amorphous germanium. Phys Status Solidi B 15:627–637. CrossRefGoogle Scholar
  41. Teja AS, Koh P-Y (2009) Synthesis, properties, and applications of magnetic iron oxide nanoparticles. Prog Cryst Growth Charact Mater 55:22–45. CrossRefGoogle Scholar
  42. Vijayaraghavan K, Ashokkumar T (2017) Plant-mediated biosynthesis of metallic nanoparticles: a review of literature, factors affecting synthesis, characterization techniques and applications. J Environ Chem Eng 5:4866–4883. CrossRefGoogle Scholar
  43. Wang SY, Lin H-S (2000) Antioxidant activity in fruits and leaves of blackberry, raspberry, and strawberry varies with cultivar and developmental stage. J Agric Food Chem 48:140–146. CrossRefGoogle Scholar
  44. Wang T, Lin J, Chen Z, Megharaj M, Naidu R (2014) Green synthesized iron nanoparticles by green tea and eucalyptus leaves extracts used for removal of nitrate in aqueous solution. J Clean Prod 83:413–419. CrossRefGoogle Scholar
  45. Wu W, Changzhong J, Roy VAL (2015) Recent progress in magnetic iron oxide-semiconductor composite nanomaterials as promising photocatalysts. Nanoscale 7:38–58. CrossRefGoogle Scholar
  46. Xiao Z, Yuan M, Yang B, Liu Z, Huang J, Sun D (2016) Plant-mediated synthesis of highly active iron nanoparticles for Cr (VI) removal: Investigation of the leading biomolecules. Chemosphere 150:357–364. CrossRefGoogle Scholar
  47. Xu P, Zeng GM, Huang DL, Feng CL, Hu S, Zhao MH, Lai C, Wei Z, Huang C, Xie GX, Liu ZF (2012) Use of iron oxide nanomaterials in wastewater treatment: a review. Sci Total Environ 424:1–10. CrossRefGoogle Scholar
  48. Zanella D, Bossi E, Gornati R, Bastos C, Faria N, Bernardini G (2017) Iron oxide nanoparticles can cross plasma membranes. Sci Rep 7:11413. CrossRefGoogle Scholar
  49. Zhang Z, Hossain MF, Takahashi T (2010) Self-assembled hematite (α-Fe2O3) nanotube arrays for photoelectrocatalytic degradation of azo dye under simulated solar light irradiation. Appl Catal B Environ 95:423–429. CrossRefGoogle Scholar
  50. Zhang H, Ji Z, Xia T, Meng H, Low-Kam C, Liu R, Pokhrel S, Lin S, Wang X, Liao Y-P, Wang M, Li L, Rallo R, Damoiseaux R, Telesca D, Madler L, Cohen Y, Zink J, Nel AE (2012) Use of metal oxide nanoparticle band gap to develop a predictive paradigm for oxidative stress and acute pulmonary inflammation. ACS Nano 6:4349–4368. CrossRefGoogle Scholar
  51. Zvarec O, Purushotham S, Masic A, Ramanujan RV, Miserez A (2013) Catechol-functionalized chitosan/iron oxide nanoparticle composite inspired by mussel thread coating and squid beak interfacial chemistry. Langmuir 29:10899–10906. CrossRefGoogle Scholar

Copyright information

© King Abdulaziz City for Science and Technology 2018

Authors and Affiliations

  • Pablo Salgado
    • 1
  • Katherine Márquez
    • 2
  • Olga Rubilar
    • 3
  • David Contreras
    • 2
    • 4
  • Gladys Vidal
    • 1
    Email author
  1. 1.Grupo de Ingeniería y Biotecnología Ambiental, Facultad de Ciencias Ambientales y Centro EULA-ChileUniversidad de ConcepciónConcepciónChile
  2. 2.Centro de BiotecnologíaUniversidad de ConcepciónConcepciónChile
  3. 3.Departamento de Ingeniería QuímicaUniversidad de La FronteraTemucoChile
  4. 4.Facultad de Ciencias QuímicasUniversidad de ConcepciónConcepciónChile

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