Noble Metal Nanoparticles: Plant-Mediated Synthesis, Mechanistic

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Noble Metal Nanoparticles: Plant Mediated Synthesis, Mechanistic Aspects of Synthesis and Applications Preeti Dauthal, and Mausumi Mukhopadhyay Ind. Eng. Chem. Res., Just Accepted Manuscript • DOI: 10.1021/acs.iecr.6b00861 • Publication Date (Web): 08 Aug 2016 Downloaded from http://pubs.acs.org on August 21, 2016

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Industrial & Engineering Chemistry Research

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Noble Metal Nanoparticles: Plant Mediated Synthesis, Mechanistic Aspects of Synthesis

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and Applications

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Preeti Dauthal and Mausumi Mukhopadhyay*

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Department of Chemical Engineering, S.V. National Institute of Technology, Surat-395007,

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Gujarat, India

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E-mail: [email protected], [email protected]; Tel: +91-261-2201645;

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Fax: +91-261-2227334, +91-261-2201641

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ABSTRACT: In recent years, the progress of efficient green chemistry approaches for

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fabrication of commercially viable noble metallic nanoparticles has become a major focus of

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researchers. The, present review has focused on the various plants mediated nanoparticle

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fabrication approaches with brief discussions on the categories of various plant mediated

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synthesis approaches and mechanistic aspects of plant mediated nanoparticle synthesis. The

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review also focused on the commercial applications of plant mediated noble metal nanoparticles.

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Significant remarks on limitation of plant mediated fabrication approaches with prospective

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future direction are also focused.

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ACS Paragon Plus Environment


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1. INTRODUCTION

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Development of nanotechnology has made a revolutionary impact in every aspect of human life.

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Nanotechnology is an interdisciplinary area of science which deals with the multi-dimensional

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aspect of nanoparticles. Nanoparticles exhibit a wide range of improved and new

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physicochemical properties that are significantly different from their bulk counterparts. The

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material particles generally show interesting and even surprising properties when they are in the

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nano-range of 1-100 nm.1 This is because, as the size of the particles approaches nano-scale, the

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percentage of atoms present at the surface of a material becomes significant and the larger

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surface area of nanoparticles dominates the contribution made by small bulk of material.2 Unique

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properties of nano-scaled materials are produced due to high surface energy, large fraction of

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surface atoms, reduced imperfections and spatial confinement.3 Nanoparticles have rewards over

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bulk materials due to their surface Plasmon light scattering, surface Plasmon resonance (SPR),

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surface enhanced Rayleigh scattering and surface enhanced Raman scattering (SERS)

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properties.4 Because of these properties, nano-scaled materials can be used as building blocks for

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various optoelectronics, electronics, chemical sensing and biological applications.5,6

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As far as fabrication of nanoparticles is concerned, metallic nanoparticles are fabricated either

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through a top-down or a bottom-up approach (Figure 1).7 In the top-down approach, metallic

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nanoparticles are fabricated through the reduction of a suitable bulk material to nano size by

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using various physical or chemical methodologies.8 In top-down approach externally controlled

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tools are utilizes for cutting, milling and shape the materials into the desired order and

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shape. Various physical synthesis methods like lithography,9 pyrolysis,10 thermolysis,11 and

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radiation induced methods,12 belongs to this category. A major shortcoming of the top-down 2


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approach is the imperfection of the surface structure of metallic nanoparticles, which exert a

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significant effect on their physical and surface chemistry properties.12 Apart from this, enormous

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consumption of energy required to maintain the high pressure and temperature during these

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synthesis procedures is the other limitation of this approach.9,12

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The bottom-up, approach is known as the self-assembly approach. In the bottom-up approach

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nanoparticles are constructed initially through the assembly of the atoms, the molecules or the

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clusters.13 The initially formed nanoparticles are then assembled subsequently into the final

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material using chemical and biological methodologies. The bottom-up approach provides a better

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chance to attain metallic nanoparticles with less surface imperfection and more homogeneous

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chemical composition at a much cheaper cost. The bottom-up approach is commonly used for

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wet synthesis procedures like chemical,14 electrochemical,15 sonochemical,16,17 and polyol

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reduction.18 Generally, the wet chemical procedures are proved to be cost effective for synthesis

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of high volume of nanoparticles.19 However, these methods also have some drawbacks. These

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methods extensively utilize toxic chemicals, nonpolar organic solvents, stabilizing and various

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synthetic capping agents in the synthesis procedures, thus prohibiting their applications in the

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clinical and biomedical domain. Extensive use of hazardous chemicals in these processes has

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raised serious concerns regarding the possible adverse effect of the chemically synthesized

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nanoparticles on the environment and living cells19,20 Replacement of wet synthesis methods by

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nontoxic, clean, reliable, biocompatible, benign and eco-friendly green chemistry methods is the

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need of the time.21 Therefore, researchers have turned their focus towards the “green” chemistry

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approaches for synthesis of metallic nanoparticles. Biofabrication of metallic nanoparticles using

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various plant systems is one such ecofriendly approach which received significant attention

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during recent years.

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Plant systems are the major photosynthetic autotrophs and first level producers in the food

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chain. These are responsible for production of high biomass in the native environment. Plant

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systems have great ability to convert light energy of the sun into chemical energy. Thus, plants

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and plant products can be utilized as renewable and sustainable resources for the fabrication of

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nanoparticles. Plants are known to harbor a wide range of antioxidant secondary metabolites.

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However, their potential is yet to be fully explored for the fabrication of metal nanoparticles. The

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use of plant resources is more beneficial over prokaryotic microbial system.22 Microbial systems

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require expensive culture maintenance approaches and downstream processing. As aforesaid,

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plants resources are a sustainable source of renewable energy and utilization of living plants,

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plant extracts or phytochemicals for the fabrication of nanoparticles is a subject of interest for

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researchers.23

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Plant mediated synthesis approach for the fabrication of metallic nanoparticles is based on the

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ability of plant system to uptake, accumulate, utilize and recycle different mineral species.24-26

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Plant mediated synthesis approach is very fast and economical for bulk production of highly

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stable nanoparticles.27 Industrial scale production of metallic nanoparticles is also possible

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through this approach by utilizing tissue culture and downstream process optimization

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techniques.28 In contrast to traditional synthesis approaches, plant mediated synthesis procedures

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have primarily used aqueous (water) extract for fabrication and require normal temperature and

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air pressure, resulting in huge energy saving.29 Plant based protocols fulfils all the criteria for

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greener synthesis. Because of these advances, the single step procedure of plant mediated 4


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synthesis has now turned as viable alternative to conventional physical, chemical, and even

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microbial methods.27,30 The key advantages of plant mediated synthesis are listed below,

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followed by detail description of each plant mediated biofabrication approaches with

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illustrations.

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Use of aqueous solvents

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Easy availability

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Biocompatible plant extracts (suitable for medicinal use)

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Simple procedure and require normal pressure and temperature (cost-effective)

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Dual role of phytoconstituents as reducing and stabilizing agent (cost-effective)

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Less or zero contamination (eco-friendly and safe for human therapeutic use)

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Suitable for large scale production

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Figure 1. General approaches for fabrication of nanoparticles. 5



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2. PLANT MEDIATED SYNTHESIS OF METALLIC NANOPARTICLES

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Biofabrication of metallic nanoparticles by plants is currently under exploration. Biosynthesis of

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metallic nanoparticles especially Au-NPs and Ag-NPs using living plants (intra-cellular), plant

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extracts (extra-cellular) and phytochemicals has received significant consideration as an

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appropriate substitute to traditional physical and chemical procedures.27 General representation

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of various plant mediated synthesis approaches is shown in Figure 2. Plant-mediated synthesis of

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metallic nanoparticles has been shown to produce nanoparticles with shapes and sizes

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comparable with those produced through traditional physical and chemical methods.31

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Figure 2. Plant mediated approaches for fabrication of nanoparticles.

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The importance and benefits of plant-mediated synthesis of nanoparticles increases many fold

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when extracts of low-cost agricultural wastes are utilized for synthesis of metallic

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nanoparticles.32 In a view to attain more control over size and morphology of nanoparticles,

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researchers are now concentrating on the use of individual phytoconstituents (e.g., polyphenols,

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proteins and organic acids) for the fabrication of metallic nanoparticles.33,34 Considering the

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importance and critical role of plants in biogenic protocols for fabrication of metallic 6


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nanoparticles, the green synthesis of metallic nanoparticles using various plant systems, probable

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mechanistic pathway, along with their commercial applications has been deliberated in this

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review.

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2.1. Living Plant or Plant Biomass Mediated Synthesis of Metallic Nanoparticles. Different

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plants species have shown pronounced potential for heavy metal accumulation (phytoextraction)

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and detoxification (phytoremediation).35,36 Considering this fact researchers today are

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concentrating more to exploit the phytoextraction and phytoremediation potential of various

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plants species for synthesis of metal nanoparticles. Gardea-Torresdey et al., (2002) have reported

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the fabrication of Au-NPs inside the living plants of Medicago sativa by gold ion uptake from

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solid media, first time in 2002.37 Later, Gardea-Torresdey et al., (2003) have also reported again

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the synthesis of Ag-NPs using living plants of M. sativa.38 Harris and Bali, (2008) have

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examined the potential of metallic silver uptake by two common metallophytes, Brassica juncea

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and M. sativa.39 They have demonstrated the potential of B. juncea and M. sativa for

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phytosynthesis of metallic Ag-NPs. In the literature, intra-cellular synthesis of metallic

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nanoparticles is scantly reported as it requires tedious and expensive processing steps to recover

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the nanoparticles from the biomass. So far, only M. sativa,37-39 B. juncea,39 Sesbania

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drummondii,40 Chilopsis linearis,41 Triticum aestivum,42 Avena sativa,43 and Festuca rubra,44 are

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reported so far to synthesize various metallic nanoparticles through intra-cellular route. The main

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constraint associated with intra-cellular route is the variation in reducing and stabilizing potential

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of bioorganic compounds available in different parts of the plant system.

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Table S1 summarizes the literature available for living plants or plant biomass mediated

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synthesis of metallic nanoparticles.37-47 Moreover, some important features of the nanoparticles 7



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defined by the U.S. Environmental Protection Agency as minimum information for nanomaterial

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characterization like size, shape, crystal structure, agglomeration (polydispersity index (PDI)),

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chemical composition, purity, surface area, surface chemistry and surface charge (ζ potential

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(mV)) are also mentioned (on the basis of existing literature).

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Table S1 clearly represented that nanoparticles are generally characterized only for size, shape

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and over all composition. Other properties related to plant mediated nanoparticles synthesis are

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scantly reported in literature. It has also been observed that highly polydispersed nanoparticles of

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diverse morphology are synthesized using single plant resource through intra-cellular route.

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Variation in functional structure and bioreducing potential of bioorganic compounds at different

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part of plant system attributed for this morphological variation and polydispersity.

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Other than the aforementioned reason, the process of metal translocation is also attributed for

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this variation. Beside this size separation and purification of nanoparticles synthesized through

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intra-cellular route is again a challenging task and this is also a contributing factor for

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morphological variation.

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It is also noticeable that despite of varying functional structure and bioreducing potential of

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bioorganic compounds at different part of plant systems, various plant systems are mostly

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favored the formation of highly reactive face centered cubic (fcc) crystalline nanoparticles.

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Though, intra-cellular route favored the formation of highly reactive nanoparticles, this approach

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is outdated now. Tedious recovery of nanoparticles from plant biomass and low commercial

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viability of plant biomass mediated nanoparticles due to associated bio-fragments has reduced

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the usefulness of this approach.

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2.2. Plant Extract Mediated Synthesis of Metallic Nanoparticles. To further simplify the

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process of metallic nanoparticle synthesis by plants, the phyto-constitutes responsible to reduce

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metal ions are extracted and utilized directly for the synthesis of metallic nanoparticles, the

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process known as extra-cellular synthesis. Researchers now prefer the extra-cellular route for

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nanoparticle synthesis because of easy downstream processing and scaling up. As compared to

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intra-cellular route, extra-cellular route of nanoparticles synthesis using plant extracts is more

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commonly studied due to their potential in several commercial applications. However, it is very

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challenging to reproduce nanoparticles with monodispersity and definite surface morphology due

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to the distinctly varying phytochemical composition and structure of plants from different

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origins. Along with this, the probability of occurrence of impurities with plant biomasses or

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agricultural wastes is always high. Therefore, it is very difficult to fabricate nanoparticles with

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desired size and morphology. It can be attained only by specific phytochemical mediated

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synthesis on a particular part of the plant biomass or living plants. This is a key aspect to be

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considererd for the synthesis of nanoparticles with high monodispersity and required surface

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morphology. Current research of biofabrication of metallic nanoparticles using plant extracts has

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opened a new era in renewable, fast, nontoxic, eco-benign and biocompatible methods for

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fabrication of nanoparticles. Many researchers have reported the biofabrication of metallic

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nanoparticles by plant extracts and their potential applications in different fields.48,49

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Table S2,52-56 S3,57-74 S4,75-152, S548,49,80,84,86,92,93,96,97,99,101,102,109,110,120,124,131,134,140,146,147,151,153-238

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summarizes the important examples of noble metallic nanoparticles (Pt-NPs, Pd-NPs, Au-NPs

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and Ag-NPs) synthesized using different plant extracts. Table S2-S5 clearly represented that the

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extra-cellular synthesis of nanostructure materials has been mainly focused on fabrication of 9



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noble metallic nanoparticles of silver and gold. Albeit, platinum and palladium are also in the

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category of noble metals, but the biofabrication of Pt-NPs and Pd-NPs, has not been explored to

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the same extent as that of Ag-NPs and Au-NPs. This is because biofabrication approaches

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generally works well for metal ions with large positive electrochemical potential.50

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Electrochemical potential of Au (1.0V) and Ag (0.80V) ions are higher as compared to the Pd

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(0.64V) and Pt (0.74V) ions. In addition, silver or gold particles are relatively inert and stable as

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compared to the other metals. Thus, these particles can be fabricated easily through biological

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routes.51 Therefore, Pd-NPs and Pt-NPs are discussed to a smaller degree as compared to the Au-

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NPs and Ag-NPs.

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It has also been observed that generally plant extract mediated synthesis support the

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fabrication of nanoparticles with more energetically favourable spherical shape and highly

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reactive fcc structure. It is well known that spherical shape and preferred growth along with

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(111) plane supports the reactivity of nanoparticles for various commercial applications. This

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observation suggests that plant extract mediated reduction is a controlled equilibrium process,

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which controlled the growth of nanoparticles up to specific shape and structure and proved the

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importance of this approach. In addition to this it is also visible in Table S2-S5 that water soluble

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polyol compounds of plant extracts are proposed as main bioreducing compounds by various

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researchers. High negative ζ potential of biosynthesized nanoparticles also proved the strong

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stabilizing potential of these water soluble polyols. High polydispersity index of plant extract

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mediated nanoparticles is also reported by many academics due to varying phytochemical

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composition of plant extract. Therefore, these observations of literature can be taken as footstep

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to go forward to focus on the individual polyols for nanoparticles fabrication. 10


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2.3. Phytochemical Mediated Synthesis of Metallic Nanoparticles. Plant extract mediated

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metallic nanoparticles synthesis generally suffers with the problem of variable phytochemical

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composition.239 Therefore it is very difficult to predict the exact mechanism of metallic

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nanoparticles synthesis using plant extracts. However, there are a few studies that predicted the

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role of polyphenols and flavonoids for synthesis and stabilization of metallic nanoparticles.33,34 In

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this context it is important to identify the exact phytoconstituents responsible for nanoparticle

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formation. Thus, researchers are focused on the isolation of particular antioxidant

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phytoconstituents for the synthesis of metallic nanoparticles. So, far only few reports available

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where phytoconstituents are directly utilized for the metallic nanoparticles synthesis as listed in

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Table S6.33,34,239-247

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2.4. Plant Mediated Synthesis of Bimetallic Nanoparticles. The synthesis of bimetallic

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nanoparticles has drawn significant consideration in the field of nanotechnology. Bimetallic

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nanoparticles also display unique optical, electronic, biological or chemical properties because of

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bi-functional or synergistic effects of monometallic counterparts.248 However, till date very few

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studies have been reported for biosynthesis of bimetallic nanoparticles. Today, most of the

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studies available are exclusively based on the synthesis of monometallic nanoparticles, excluding

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few examples as listed in Table S7.248-258

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3. POSSIBLE MECHANISM OF PLANT MEDIATED NANOPARTICLE SYNTHESIS

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Fabrication of nanoparticles required mainly three constituents such as reducing agents,

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stabilizing agents and solvent medium.259 During plant extracts mediated metallic nanoparticles

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synthesis, phytoconstituents of plant extracts plays the dual role as reducing and stabilizing

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agent. Generally plant mediated synthesis of metal nanoparticles is required aqueous medium

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and regarded as a green process. Nowadays, biosynthesis of nanoparticles using plant systems is

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under extensive research. However, specific mechanism for the plant mediated synthesis of

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nanoparticles has not yet been interpreted well. Till now, various hypothetical mechanisms have

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been suggested for plant mediated synthesis of metallic nanoparticles.13,260 Due to complex

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nature and huge variety of phytochemicals present in plant extract, it is a challenging mission to

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recognize a specific bioreducing and stabilizing agent responsible for the fabrication and

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stabilization of nanoparticles. Till now, phytoconstituents such as polyphenols (flavonoids,

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phenolic acid and terpenoids), organic acid and proteins are considered as probable bioreducing

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and stabilizing agents for fabrication of nanoparticles. However, it is very likely that for

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bioreduction reaction of metallic ions, several phytoconstituents of plant extracts act

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synergistically.119 Sathishkumar et al., (2009) has also supported that polyols (terpenoids and

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flavones) and polysaccharide contents of C. zeylanicum extract act together for the reduction of

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metallic ions.261 The detail of how each of the phytoconstituents take part as bioreducing and

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stabilizing agents in plant mediated nanoparticles synthesis is deliberated in following sections.

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3.1. Flavonoids. Flavonoids are water-soluble plant secondary metabolites. Flavonoids contain

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15 carbon atoms. Flavonoids comprise 6 major subgroups: anthoxanthins, flavanones,

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flavanonols, flavans, anthocyanidins and isoflavonoid. Flavonoids are supposed to be the key 12


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bioreducing constituents of aqueous plant extracts. The molecular oxygen scavenging

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(antioxidant or reducing) potential of flavonoids is directly related to their electron or hydrogen

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atoms donation ability.262,263

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The hydrogen and electron releasing capability of flavonoids is well exploited nowadays for

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fabrication of metallic nanoparticles by different researchers.264-268 Hence, flavonoids contents of

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plant extracts are now being utilized as an important indicator for preliminary evaluation of

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unexploited plants for synthesis of metallic nanoparticles.103 Ahmad et al., (2010) suggested that

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free hydrogen liberated during keto-enol conversion of flavonoids (luteolin and rosmarinic acid)

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are responsible for the reduction of metal ions to corresponding nanoparticles.216 Similarly,

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Ghoreishi et al., (2011) suggested that the hydroxyl groups of flavonoids (quercetin and

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myricetin) are oxidized to carbonyl groups during bioreduction of metal ions.80

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3.2. Phenolic Acid. Phenolic acids belong to the family of polyphenols. Phenolic acid contains

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a phenolic ring and an organic carboxylic acid function. Antioxidant activities of these

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compounds are related to the metal chelating ability of highly nucleophilic aromatic rings of

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phenolic acid.269 Various type of plant phenolic acids namely, gallic acid,270 caffeic acid,138

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ellagic acid,229 and protocatechuic acid,87 are reported as bioreducing agents for the fabrication

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of metallic nanoparticles. Supporting these conclusions, few researchers have directly utilized

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gallic acid for the reduction of metal ions and metal reducing potential of gallic acid has been

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proved in literature.266,269 Edison and Sethuraman, (2012) have suggested that synthesis of Ag-

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NPs takes place due to the formation of an intermediate complex of silver ions with phenolic

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hydroxyl groups of gallic acid, which consequently undergo oxidation to quinone with

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subsequent reduction of silver ions to Ag-NPs.229 13



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Aromal et al., (2012) has stated that the hydrogen released during the transformation of caffeic

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acid to ferulic acid is responsible for the bioreduction of gold ions.138 Caffeic acid displays strong

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reducing activity because of additional conjugation in the propanoic side chain. This facilitates

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the electron delocalization, by resonance, between the aromatic ring and propanoic group. The

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metal reducing potential of a few other polyphenolic compounds such as lignan (phyllanthin),244

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flavonoid glycosides (apiin),245 and tannin (bayberry tannin),270 are also reported in the literature.

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The polyphenolic compounds are capable to chelate many kinds of metallic ions (Pt4+, Au3+, Pd2+

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and Ag+ etc.) through their dense ortho-phenolic hydroxyls groups.271 Hence these compounds

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act as reducing agents for the fabrication of metallic nanoparticles.

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3.3. Terpenoids. Terpenoids (isoprenoids) are a large and diverse class of naturally occurring

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small molecular weight organic compounds synthesized by plants, which belong to the category

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of terpenes. Terpenoids are responsible for the aroma, taste and color of various plant species.

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Shankar et al., (2003) has reported the ability of hydroxyl functional groups of terpenoids

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(citronellol and geraniol) present in P. graveolens leaf extract for the bioreduction of silver

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ions.122 Later, Safaepour et al., (2009) has also proved the role of geraniol for the synthesis of

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Ag-NPs.247 Similarly, terpenoid contents of C. zeylanicum bark extract such as linalool, eugenol

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and methyl chavicol are also reported for metal reducing potential.261 Singh et al., (2010) has

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suggested the role of eugenol of S. aromaticum extract as a bioreducing agent for fabrication of

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Au-NPs and Ag-NPs.242 Eugenol transforms itself to its anionic form due to proton releasing

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ability of the hydroxyl group of eugenol. Furthermore, the reducing power of eugenol is

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significantly improved due to the inductive effect induced by the electron withdrawing methoxy

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and allyl functional groups present at the para and ortho positions of the hydroxyl group. The 14


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two electrons released simultaneously during the reaction are responsible for the reduction of

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metal ions.

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3.4. Proteins. Protein mediated bioreduction is complicated due to their complex structure. It is

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well known that nanoparticles can bind to proteins through their free amino or carboxylate

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groups.103 Interaction of silver ions with arginine, cysteine, lysine and methionine residues was

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also reported earlier.272 Tan et al., (2010), have tested the reducing and binding ability of twenty

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amino acids with metal ions.273 Bioreducing and capping role of cyclic peptides present in the

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latex of J. curcas has also been proved for synthesis of Ag-NPs.163 Roy et al., (2014) has

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recently described the reducing potential of tyrosine for metal ions of silver, through the

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ionization of the phenolic group in tyrosine. This leads to the formation of the semi-quinone

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structure of tyrosine.274 The metal reducing potential of tyrosine was also proved by other

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researchers.275,276 Wangoo et al., (2008) has verified the single step synthesis of metallic

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nanoparticles by complex formation with glutamic acid.277 One other amino acid tryptophan is

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also reported to have reductive properties by the release of an electron during conversion of the

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tryptophan residue to a transient tryptophyl radical.278,279

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3.5. Organic Acids. Plant systems are capable to produce a diverse range of secondary

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metabolites upon exposure to various metals. Various secondary metabolites such as organic

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acids and alkaloids are reported as bioreducing agents for the fabrication of different metallic

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nanoparticles. Tamuly et al., (2014) have stated the metal reducing potential of a plant alkaloid

20

(pedicellamide) isolated from P. pedicellatum.34 Pedicellamide exert metal reducing potential

21

through the release of reactive hydrogen. The role of ascorbic acid of C. sinensis peel extract is

22

also reported as an effective reducing agent for the synthesis of Ag-NPs.206 15



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Page 16 of 87

1

Jha et al., (2009) has reported the metal reducing potential of the different plant species from

2

mesophyte, hydrophyte and xerophyte genera.28 Tautomerization of benzoquinone derivatives

3

has been reported to contribute to the metal reducing capability of the Cyperus sp. of mesophyte

4

genera. Similarly, in hydrophyte genera, compounds such as protocatecheuic acid, catechol and

5

ascorbic acid of Hydrilla sp. have been reported to release reactive hydrogen. This reactive

6

hydrogen contributed to the bioreduction of metallic silver ions. In xerophyte genera, pyruvic

7

and malic acid produced during the redox reaction of glycolytic pathway in Bryophyllum sp.

8

leads to the reduction of metallic silver ions.28 The keto-enol tautomerization of emodin in

9

xerophytes (anthroquinones derivative) is also known for the reduction of metal ions.

10

4. APPLICATIONS OF PLANT MEDIATED NANOPARTICLES

11

Nanoparticles of gold, silver, platinum and palladium metals are extensively used nowadays to

12

satisfy the needs of fast-growing consumer world.280 There is growing need to fabricate eco-

13

friendly and biocompatible nanoparticles. Biologically synthesized nanoparticles are reported to

14

have less compatibility issues with cells of living systems, particularly when used for medical

15

applications as compared to traditionally synthesized nanoparticles.265,268 Despite wide

16

applicability of biosynthesized nanoparticles in various domains, the polydispersity of the

17

nanoparticles formed during biosynthesis reactions remains a challenge. This critical aspect of

18

polydispersity is crucial to be considered for biosynthesized nanoparticles to improve their

19

performance in various domains. In recent years many researchers have therefore tried to

20

establish a stable system for fabricating nanoparticles with significant homogeneity in terms of

21

morphology and size. Various researchers have tried to attain homogeneity either by controlling

22

process parameters of biosynthesis reaction or by altering and isolating the bioreducing 16


Page 17 of 87

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1

molecules (phytoconstituents). For instance, Kora et al., (2012) has reported the process

2

parameter controlled Anogeissus latifolia mediated synthesis of nearly monodispersed and

3

spherical nanoparticles of around 5.7 ± 0.2 nm.281 Ghodake et al., (2010) and Sathishkumar et

4

al., (2010) has demonstrated that pH is a key factor for controlling the size and morphology of

5

nanoparticles as pH influenced the charge of natural phytoconstituents.85,221 This further affects

6

binding ability and reduction potential of phytoconstituents and ultimately leads alterations in the

7

morphology and size of nanoparticles and finally yield of bioreduction reaction. Beside pH,

8

various other parameters like concentration of metal ion and plant extract, ratio of plant extract to

9

metal ion, exposure time and reaction temperature are also determining factors for nanoparticles

10

homogeneity.103,110,120,303 By varying one or many factors, one can prepare nanoparticles with

11

significant homogeneity and high stability.27,110,303

12

It is well known that high polydispersity of plant mediated nanoparticles is also due to the

13

varying phytochemical composition of plant extracts. To overcome this issue and to get more

14

control over shape and size of biosynthesized nanoparticles many researchers are now focusing

15

on pure phytoconstituent for nanoparticles synthesis.33,34 To justify this, Roy et al., (2010) has

16

compared the bioreduction behavior of two flavonoids (pinocembrin and galangin) of Indian

17

propolis with their parent material (aqueous extract of Indian propolis).282 More homogeneous

18

size distribution was observed in flavonoids mediated nanoparticles as compared to the aqueous

19

extract mediated nanoparticles. Aqueous extract of Indian propolis is a mixture of many

20

bioreducing compounds with different reducing properties. Therefore, it is clear that the pure

21

flavonoids are more capable to form nanoparticles with high monodispersity than the aqueous

22

extract.282 Ahmed et al., (2014) also supported this observation that β-sitosterol-D17



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1

glucopyranoside produced nanoparticles with higher negative ζ potential (-15.9 mV) as

2

compared to the parent material (aqueous extract of D. bipinnata) mediated nanoparticles (12.5

3

mV), suggested higher stability of pure phytoconstituent mediated nanoparticles.239

Page 18 of 87

4

As far as separation and purification of plant mediated nanoparticles is concerned, multi-steps

5

high-speed centrifugation (based on gravitational force) is a traditional approach to remove un-

6

coordinated plant molecules from the colloidal solution.205,244 However, this technique is not

7

suitable for separation of tightly coordinated phytochemicals of nanoparticles surface, which can

8

further influence the biocompatibility aspects of biofabricated nanoparticles. Therefore, size-

9

based separation and purification of biofabricated nanoparticles still remain as a major challenge.

10

Therefore, production of well-defined nanoparticles for the purpose of application and

11

fundamental research is still facing the problem of polydispersity. During recent years,

12

techniques like ion exchange based chromatography and electric charge based electrophoresis

13

are also used for purification and size separation of water-soluble nanoparticles.283,284 However,

14

the separation of water-soluble nanoparticles from impurities is particularly difficult because of

15

the similar solubility index. So these purification techniques are also proved inefficient.

16

Sweeney et al., (2006) introduce recently a new technique named diafiltration for effective

17

size-based separation and purification of water-soluble nanoparticles.285 Diafiltration is a single

18

step process for the isolation of smaller nanoparticles from larger nanostructures. This technique

19

is also efficient for the removal of small-molecule impurities. Diafiltration produces

20

nanoparticles with a much higher degree of purity as compared to the other processes like

21

dialysis or a combination of solvent washes, chromatography and ultracentrifugation.

18


Page 19 of 87

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1

The present review has been taken into account a few applications where biosynthesized

2

nanoparticles are used for various biomedical, industrial and environmental applications. The

3

key biomedical applications of biosynthesized metallic nanoparticles reviewed here are

4

antimicrobial,49 antifungal,65 antiparasitic,155 and anticancer activity.83 The nanoparticles applied

5

for environmental remediation activity include reduction of toxic environmental pollutants such

6

as nitro-organic compounds and dyes. Industrial applications of nanoparticles reviewed here

7

include the use of biosynthesized nanoparticles as catalysts for commercially important organic

8

synthesis reactions such as hydrogenation,49 cross-coupling,68 and oxidation.250 The present

9

review is organized according to the various applications of plant derived noble metallic

10

nanoparticles broadly classified into biomedical, environmental and industrial applications.

11

4.1. Biomedical Applications. There are various applications of metal nanoparticles reported in

12

the domain of biomedical sciences. These nanoparticles still have significant potential for

13

continual growth in various areas of biomedical science. Metallic nanoparticles are widely

14

applied for antibacterial,49 antifungal,65 and insecticidal functionality.155 Because of these

15

properties, metallic nanoparticles are incorporated into surgical implants, topical ointments,

16

creams, wound dressings, bone cements, medical devices and ultrasound gels.286,287 In addition,

17

they are also utilized in food processing.288 Recently, metallic nanoparticles have also been

18

reported for use in cell imaging,194 therapeutic,256 and targeted drug delivery289 applications

19

because of their medically relevant optical,290 cytotoxic,291 surface Plasmon light scattering and

20

surface Plasmon absorption properties.292

21

4.1.1. Antimicrobial Applications. Due to on-going evolution of multi-drug resistance traits in

22

different microbial systems, the development of new antimicrobial agents is essential. Due to the 19



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Page 20 of 87

1

remarkable antimicrobial potential of noble metallic nanoparticles, particularly silver and gold,

2

they are well employing nowadays as antibacterial, antifungal and antiviral agents.293 The

3

following sections define the key antibacterial and antifungal properties of plant mediated

4

metallic nanoparticles reported in the literature.

5

The exact mechanism of nanoparticles mediated antimicrobial activity is not clearly known.

6

However, various possible mechanisms are discussed in the literature for the antimicrobial effect

7

of nanoparticles. Sondi and Salopek-Sondi, (2004) have proposed the anchoring ability of

8

nanoparticles towards the bacterial cell wall, which leads penetration to the bacterial cell wall.

9

This finally causes structural changes in the cell membrane and form ‘pits’ on the cell surface.

10

Accumulation of nanoparticles under the surface of bacterial cell through the pits of the cell

11

surface is considered the other reason of antimicrobial activity.294 The ability of nanoparticles to

12

generate free radicals is deliberated as another mechanism by which bacterial cells die. Free

13

radicals create porosity in the cell membrane, which leads the cell membrane damage and cell

14

death.295 It has also been proposed that interaction of silver ions (released from Ag-NPs) with

15

thiol groups of numerous bacterial enzymes inactivated them.296,297 The interaction of Ag-NPs

16

with the sulfur and phosphorus groups of bacterial DNA has also been proposed to interfere with

17

bacterial DNA replication and finally terminate the microbial system.298 Interference of signal

18

transduction in bacteria through phosphorylation of protein substrates is also accounts for

19

antibacterial action of nanoparticles.299 The generalized scheme of plausible antimicrobial

20

activity of nanoparticles is illustrated in Figure 3. However, further research is required to prove

21

the exact mechanisms through nanoparticles exert antimicrobial activity.

20


Page 21 of 87

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1 2

Figure 3. Modes of nanoparticles mediated antimicrobial activity.

3

Till now, large number of research groups focused on the antibacterial activity of metallic

4

nanoparticles as compared to their antifungal and antiviral activity. This is due to the fact that

5

nanoparticles at low concentration never enter into the fungal cells, but easily adsorbed onto the

6

bacterial surface. This further blocks the respiration across the cell membrane of the bacteria.

7

However, respiration occurs through the mitochondrial membrane in eukaryotic cells of fungi.300

8

Similarly, there have been only few reports available on antiviral activity of biofabricated

9

metallic nanoparticles.301 Viruses causes severe complications in agriculture and medicine.

10

Therefore, efforts made in this direction will certainly highlight a possible therapeutic dimension

11

of nanoparticles. Very few reports demonstrate the size-dependent interaction of Ag-NPs with

12

herpes simplex, human parainfluenza and human immunodeficiency viruses.302,303 Murugan et

13

al., (2015) reported the antiviral effect of B. cylindrical mediated Ag-NPs. B. cylindrical

14

mediated Ag-NPs significantly inhibited the production of dengue viral envelope (E) protein in

15

viral cells and downregulated the expression of dengue viral E gene, which ultimately produced 21



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Page 22 of 87

1

antiviral effect.157 Representative examples are provided here to summarize the overall potential

2

of plant mediated nanoparticles against a wide range of bacterial (Tables 1) and fungal (Table 2)

3

systems.

4

Table 1. Antibacterial activity of plant mediated nanoparticles Nanoparticles Ag49 Au90 Au and Ag124 Au137 Au and Ag146 Ag152 Ag153 Ag154 Ag162 Ag188 Ag203 Ag204 Ag210 Ag212 Ag221 Ag286 Ag304 Ag305 Ag306

Plant resources S. brachiate A. comosus A. occidentale C. zeylanicum M. piperita C. religiosum S. potatorum C. asiatica D. bulbifera C. murale H. cannabinus C. siliqua T. chebula M. indica C. longa Chrysanthe mum morifolium A. indica O. tenuiflorum S. grandiflora

Applications Staphylococcus aureus, Bacillus subtilis subtilis and Escherichia coli E. coli and Streptobacillus flavus Aeromonas hydrophila, Aeromonas bestiarum and Pseudomonas fluorescens E. coli and S. aureus S. aureus and E. coli E. coli, Proteus vulgaris, Pseudomonas aeruginosa and B. subtilis S. aureus and Klebsiella pneumoniae S. aureus, B. subtilis, E. coli and P. aeruginosa E. coli S. aureus E. coli, Proteus mirabilis and Shigella flexneri E. coli S. aureus and E. coli E. coli, S. aureus and B. subtilis on non-woven fabrics E. coli on cotton fabrics S. aureus and E. coli on ultrasound gel

S. aureus and E. coli on cotton fabrics E. coli, Corney bacterium and B. substilus Salmonella enterica and S. aureus

5 6 22


Page 23 of 87

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1


Table 2. Antifungal activity of plant mediated nanoparticles Nanoparticles Pd65 Au129 Au137 Ag152 Ag159 Ag166 Ag307 Ag308 Ag309 Ag310

Plant resources Applications P. betle Aspergillus niger A. esculentus Puccinia graminis, Aspergillus flavus, A. niger and Candida albicans C. zeylanicum A. niger and Fusarium oxysporum C. religiosum A. niger, A. flavus, Fusarium sp., Curvularia sp. and Rhizopus sp. A. vera Rhizopus sp. and Aspergillus sp. S. arvensis Neofusicoccum parvum A. indica Alternaria alternata, Sclerotinia sclerotiorum, Macrophomina phaseolina, Rhizoctonia solani, Botrytis cinerea and Curvularia lunata Gelidiella Humicola insolens, Fusarium dimerum, Mucor indicus and acerosa Trichoderma reesei Sesuvium A. alternata, Penicillium italicum, Fusarium equisetii and C. portulacastrum Albicans C. limon F. oxysporum and Alternaria brassicicola on fabrics

2 3

4.1.2. Antiparasitic Applications. Biofabricated nanoparticles are effective against numerous

4

disease-causing parasites or insects. The antiparasitic effect of nanoparticles depends on their

5

membrane penetration ability. Nanoparticles induce a distress in proton motive force. Proton

6

motive force is required for ATP construction. This disturbance leads loss of cellular function

7

and finally cell death.311 Binding of nanoparticles in the intracellular space with sulphur-

8

containing proteins and phosphorus-containing DNA, also leads denaturation and structural

9

deformation. Structural deformation created by nanoparticles also accounts for the anti-parasitic

10

effect of nanoparticles.293,294 A synergistic combination of nanoparticles with proteins,

11

polyphenols and other secondary metabolites adhering on the surface of plant mediated

12

nanoparticles accounts for increased larvicidal spectrum of plant mediated nanoparticles. The

23



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1

ability of various plant system mediated nanoparticles against a wide spectrum of parasites has

2

been validated by different research groups and cited in Table 3.

3

Table 3. Antiparasitic activity of plant mediated nanoparticles Nanoparticles Ag155 Ag157 Ag158 Ag185 Ag199 Ag201 Ag312

Plant resources D. metel B. cylindrical C. roxburghii N. nucifera R. mucronata M. zapota M. paradisiaca

Ag313 Ag314

C. nucifera Pithecellobium dulce L. inermis

Ag315

Page 24 of 87

Applications Anopheles stephensi Aedes aegypti A. stephensi, A. aegypti and Culex quinquefasciatus Anopheles subpictus and C. quinquefasciatus A. aegypti and C. quinquefasciatus Rhipicephalus microplus Haemaphysalis bispinosa, Hippobosca maculate, A. stephensi, Japanese encephalitis and Culex tritaeniorhynchus A. stephensi and C. quinquefasciatus C. quinquefasciatus Pediculus humanus capitis and Bovicola ovis

4 5

4.1.3. Anticancer Applications. Anticancer potential of biosynthesized nanoparticles have been

6

reported against various cancer cell lines as listed in Table 4. Nanoparticles exert anticancer

7

potential against various cancer cell lines through apoptosis,150 anti-proliferative,187 anti-

8

metastatic,316 and cytotoxic317 effect. Cytotoxic and caspase-mediated apoptotic effect of plant

9

mediated nanoparticles is reported against human cervical carcinoma cells through the

10

generation of reactive oxygen species (ROS). ROS create imbalance in the intrinsic apoptotic

11

pathway centred at mitochondria by modulation of Bax and Bcl-2 expressions. They, induced

12

cell death by caspase dependent pathway.169

13

Anti-proliferative activity of bio-functionalized nanoparticles is also reported in the literature

14

against various cancer cell lines through the generation of free radicals.187 Free radicals

15

contributes to electron propagation all around the cancer tissues. This causes shrinkage and 24


Page 25 of 87

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1

rupture of the cell surface followed by improper nutrient and signal supply and ultimately cell

2

death. Recently, the anti-metastatic activity of biofabricated nanoparticles has also been

3

described for the human fibrosarcoma cell line HT-1080 by interfering with the actin

4

polymerization pathway.316

5

Cytotoxic effect of P. longum mediated nanoparticles is also identified due to the formation of

6

superoxide, hydrogen peroxide and hydroxyl radicals. These free radicals cause damage to the

7

cellular components such as proteins lipids and DNA. This eventually leads to cell death.175

8

Presence of surface adsorbed bioorganic moieties at the surface of plant mediated nanoparticles

9

has a synergistic effect on anticancer potential of nanoparticles.289

10

Table 4. Anticancer activity of plant mediated nanoparticles Nanoparticles Au83 Au91

Plant resources Applications C. guianensis Cytotoxicity on HL-60 cells lines P. granatum Cytotoxicity for breast cancer lines MCF-7

Au106 Au and Ag109

T. nucifera, C. japonicum and N. indicum A. indica

Ag149

P. hexandrum

Au150

L. montevidensis P. longum S. grandiflora A. sessilis C. colocynthis V. negundo C. collinus T. baccata P. guajava

Ag175 Ag182 Ag187 Ag190 Ag196 Ag237 Ag238 Au288

Cytotoxicity for 3T3-L1 cell lines

Cytotoxic activity for MDA-MB-231 human breast cancer cells Cytotoxicity and caspase-mediated apoptotic effect on human cervical carcinoma cells Apoptosis effect in lung (A549), breast (MCF-7) and melanoma (B16) cancer cells Cytotoxic activity against Hep-2 cell lines Anticancer efficiency for breast cancer cells Anti-proliferative effect on prostate cancer cells Cytotoxic effect on Hep-2 cells Cytotoxic effect against human colon cancer cell lines Cytotoxicity on human lung cancer cells lines A549 Anticancer effects on MCF-7 cells Cytotoxic activity against HEK-293, HeLa and HT-29 cells lines To be continued… 25



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Nanoparticles Au316 Ag317 Ag318 Ag319 Ag320 Ag321 Ag322 Ag323 Au324 Au325

Plant resources Dysomsa pleiantha M. citrifolia Albizia adianthifolia Ficus religiosa Melia azedarach Erythrina indica Origanum vulgare Phyllanthus emblica Fagopyrum esculentum Vites vinefera

Page 26 of 87

Applications Anti-metasatic activity against human fibrosarcoma cell lines HT-1080 Cytotoxic effect on HeLa cell lines Cytotoxic effect on A549 lung cell lines Apoptosis effect on dalton ascites lymphoma Cytotoxic activity against HeLa cell lines Cytotoxic effect on MCF-7 and HEP G2 cell lines Cytotoxicity on human lung cancer cell lines A549 Anti-proliferative effect on Hep2 cell lines Cytotoxic activity against HeLa, MCF-7 and IMR-32 cancer cell lines Cytotoxic activity against HBL-100 cells

1

4.1.4. Antioxidant Applications. Free radicals are known to be responsible for the development

2

of many pathological conditions ranging from cancer to cardiovascular disease, Alzheimer’s

3

disease, atherosclerosis, diabetes and aging.326,327 So, evaluation of the free radical scavenging

4

potential of biosynthesized nanoparticles may be beneficial for the treatment of various free

5

radical associated medical conditions and further explore their wide range of medically relevant

6

properties. During recent years, the in-vitro free radical scavenging potential of biogenic

7

nanoparticles and their association for the treatment of various pathophysiological conditions are

8

demonstrated by various researchers.233-236 Literature demonstrates the antioxidant potential of

9

biogenic nanoparticles for scavenging of free radicals and treatment of associated medical

10

conditions as listed in Table 5.

11 12

26


Page 27 of 87

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1


Table 5. Free radical scavenging activity of plant mediated nanoparticles Nanoparticles Ag48

Plant resources A. sessilis

Ag49 Au and Ag84

S. brachiata P. armeniaca

Au139 Au and Ag140

S. nigrum S. torvum

Ag159 Ag206 Ag233

C. banana C. sinensis S. cumini

Ag234

P. longum

Ag235

I. herbstii

Ag236

A. paniculata

Ag237

C. collinus

Applications 1,1-diphenyl-2-picryl hydroxyl radical (DPPH•) scavenging DPPH• scavenging DPPH• and 2,2-azinobis-(3-ethylbenzothiazoline-6sulfonic acid radical (ABTS•+) scavenging DPPH• and hydroxyl radical scavenging DPPH•, hydroxyl, superoxide and nitric oxide radical scavenging activity with DNA protection activity DPPH• and ABTS•+ scavenging DPPH• scavenging and anti-lipid peroxidation activity DPPH• and ABTS•+ scavenging with anticancer activity against dalton lymphoma cells DPPH•, superoxide, nitric oxide and hydrogen peroxide scavenging activity with cytotoxic effect against MCF-7 breast cancer cell lines DPPH• scavenging, reducing power activity with cytotoxic activity against HeLa cervical cell lines DPPH• scavenging activity associated with curative effects on liver injuries caused by CCl4 DPPH•, hydroxyl and hydrogen peroxide scavenging activity with cytotoxicity against human lung cancer cells 31

2 3

4.1.5. Other Medical Applications. Biocompatibility of nanoparticles with cells of human

4

system is an important concern for in-vivo applications. Moulton et al., (2010) has carried out

5

ultra-resolution microscopy and mitochondrial function test for evaluating the effect of

6

biosynthesized Ag-NPs on human keratinocyte cells.265 Ag-NPs have not posed any effect on

7

cell viability and membrane integrity of human keratinocyte cells. These results showed that

8

biosynthesized Ag-NPs are nontoxic and biocompatible. The biocompatibility of biosynthesized

9

Ag-NPs may be attributed to the antioxidant effect of polyphenols and flavonoids surfactants

10

present in tea extract. Lee et al., (2011) proved the excellent cytoprotective and biocompatibility 27



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Page 28 of 87

1

properties of antioxidant phytochemical-capped Au-NPs for L-929 fibroblastic cells.268 Kumar et

2

al., (2011) has described the compatibility of Z. officionale mediated Au-NPs for human blood

3

cells, also suggested these nanoparticles as possible candidates for various therapeutic

4

applications.126 Hemocompatibility of P. granatum mediated Au-NPs is also proved earlier for

5

human blood samples.91 Anti-angiogenic activity of A. biebersteinii mediated Ag-NPs also

6

reported for rat aortic ring model.168

7

Several studies have shown the potential of biosynthesized nanoparticles for the treatment of

8

various diseases. In-vitro anti-diabetic potential of P. guajava mediated Au-NPs have already

9

been reported which act by inhibiting the enzyme tyrosine phosphatase type PTP 1B, responsible

10

for dephosphorylate of insulin receptors.33 Similarly, Venkatachalam et al., (2013) has used

11

functionalized Au-NPs as an anti-diabetic nanomaterial.328Another study showed that the

12

antioxidant activity of biosynthesized Ag-NPs has played a crucial role for the curative effect on

13

the hepatic injury induced by CCl4.236 The positive implications of O. tenuiflorum mediated

14

colloidal Ag-NPs on haematological and biochemical functions of freshwater fish Labeo rohita,

15

proved the prominent immunomodulatory effect of biosynthesized nanoparticles.202 Singh et al.,

16

(2010) has reported the functionalization of biosynthesized Au-NPs with -NH2 group of L-

17

cysteine moiety and suggested their role for various biological applications like drug delivery,

18

imaging, clinical diagnosis and for trans-locating therapeutic molecules.242 Das et al., (2013) has

19

proved the applicability of green synthesized quercetin functionalized Au-NPs in chemotherapy

20

of wild and drug resistant type visceral leishmaniasis with a very high selectivity index.329 Wang

21

et al., (2007) suggested, gallic acid mediated Au-NPs as an excellent precursor material for the

22

preparation of thiol-modified biological probes which can be used for various biological 28


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1

analyses.269 Sarkar et al., (2010) has reported the labelling and imaging applications of P.

2

hysterophorus mediated Ag-NPs.224

3

4.2. Catalytic Applications for Environmental Remediation. Due to large surface area per

4

volume ratio, high selectivity, activity and stability of metallic nanoparticles, nanoparticles are

5

widely used as catalysts for various environmental remediation reactions such as catalysts for the

6

removal of various toxic environmental pollutants.

7

4.2.1. Catalytic Reduction of Nitro-Organic Pollutants. The rapid increase in the use of nitro-

8

organic compounds for the manufacturing of pharmaceuticals, plasticizers, dyes, fungicides,

9

pesticides and explosives results in their continued release in soil and water.330 These

10

anthropogenic compounds are highly perilous on release in the environment and are known as

11

‘‘priority pollutant’’ by US Environmental Protection Agency (US-EPA). Due to their high

12

solubility and stability index in the aqueous environment, these compounds stay longer time in

13

water and soil surfaces. Public health hazards are also reported because of ingestion of these

14

nitro-organic pollutants.331-333 In a view of environmental remediation and safety of public

15

health, many researchers are focused on the sodium borohydride mediated reduction of various

16

nitro-organic pollutants using biosynthesized nanoparticles as catalysts as listed in Table 6.

17

The catalytic activity of the biosynthesized nanoparticles is possibly due to the efficient

18

electron transfer from BH4- ion to nitro-organic compounds. This is attributed to the higher

19

driving force of nanoparticles-mediated electron transfer caused by their large Fermi level shift

20

in the presence of highly electron-injecting borohydride ions. These reactions are reported at

21

room-temperature and in an aqueous medium. Thus, biosynthesized nanoparticles can be utilized

22

for the treatment of industrial toxic wastewater containing nitro-organic effluents. 29



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1

Page 30 of 87

Table 6. Plant mediated nanoparticles for catalytic reduction of nitro-organic pollutants Nanoparticles Au40 Ag49 Pt55 Pt56 Pd74 Au89 Au and Ag96 Au104 Au107 Au112 Au121 Ag and Au131 Au132 Au142 Au143 Au144 Au145 AuPd255 AuAg258

Plant resources S. drummondii S. brachiate A. occidentale P. granatum D. regia P. domestica C. aurantifolia S. brachiata P. dactylifera A. nilotica A. occidentale B. rhamnoides C. nucifera S. mukorossi T. foenumgraecum P. granatum M. oleifera D. regia S. marianum

Applications Reduction of 4-nitrophenol (4-NP) Reduction of 4-NP Reduction of 4-NP Reduction of 3-nitrophenol (3-NP) Reduction of 2-nitrophenol (2-NP) and 2-nitroaniline (2-NA) Reduction of 4-NP Reduction of 4-nitroaniline (4-NA) Reduction of 4-NP Reduction of 4-NP Reduction of 4-NP Reduction of 4-NP Reduction of 4-NP Reduction of 4-NP Reduction of 4-NA Reduction of 4-NP Reduction of 4-NP Reduction of 4-NP and 4-NA Reduction of 3-nitroaniline (3-NA) Reduction of 4-NP

2 3

4.2.2. Catalytic Reduction of Dyes. The widespread use of organic dyes in the cosmetics,

4

textile, paper, food and pharmaceutical industries causes the serious pollution problem for the

5

environment through industrial effluent. Several remediation processes are used for reduction of

6

these organic dyes.334,335 Due to high stability and complex structure of dye molecules, it is very

7

difficult to degrade or remove these dyes from industrial effluents. Therefore, in the present

8

scenario, scientists have shown considerable interest in using biosynthesized metallic

9

nanoparticles for the degradation of dyes. Biosynthesized nanoparticles as catalysts have been

10

used successfully for the degradation of different organic dyes as listed in Table 7. 30


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1


Table 7. Plant mediated nanoparticles for catalytic reduction of organic dyes Nanoparticles Pd72 Au104 Au141 Ag179 Ag227

Plant resources C. roseus S. brachiata S. grandiflora P. pedicellatum C. grandis

Ag228 Ag229 Ag230 Ag231

U. lactuca T. chebula F. panda T. foenumgraecum L. martinicensis

Ag232

Applications Photocatalytic degradation of phenol red Reduction of methylene blue Reduction of methylene blue Photocatalytic degradation of methyl red Photocatalytic degradation of coomassie brilliant blue G250 Photocatalytic degradation of methyl orange Reduction of methylene blue Reduction of methylene blue Catalytic degradation of methyl orange, methylene blue and eosin Y Reduction of methylene blue

2 3

It is well known that catalytic potential of nanoparticles depend on their size. Metals in bulk

4

form are chemically inert because of their redox potential.336 Haruta, (1989) has reported that

5

metallic gold becomes catalytically active at the nano-level due to the reduction of its redox

6

potential to negative.337 The redox potential of an efficient catalyst is between the redox potential

7

of the donor and the acceptor system.338 On the basis of above mentioned fact, various

8

researchers have proposed that biosynthesized nanoparticles act as an electron transfer mediator

9

between donor (plant extract) and acceptor system (organic dyes) by acting as a redox catalyst.

10

This process is known as an electron relay effect.229,230

11

4.3. Industrially Important Applications. Use of low-cost specific catalysts for commercially

12

valuable organic synthesis reactions such as hydrogenation, oxidation, cross-coupling, reduction

13

and epoxidation are very important in industries. During recent years, biosynthesized

14

monometallic nanoparticles along with bimetallic nanoparticles have been used effectively as

15

catalysts in several organic synthesis pathways as mentioned in Table 8. Biosynthesized A. 31



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1

annua mediated Pd-NPs have been used as catalyst for the synthesis of biologically interesting

2

di(indolyl)indolin-2-one dyes from isatin and indole in water. Reusability study demonstrated

3

that Pd-NPs retained its activity for five consecutive cycles.62 C. platycladi mediated Pt-NPs also

4

utilized as catalyst for hydrogenation of cinnamaldehyde to commercially important cinnamyl

5

alcohol, which is utilized as a raw material and an intermediate for a wide range of formulations

6

for use as medicines, bactericides, fragrances, cosmetics and pesticides.339 In addition to this,

7

bimetallic biosynthesized nanoparticles are often introduced as catalysts for various industrial

8

applications.248,250

9

Table 8. Plant mediated nanoparticles as catalyst for organic synthesis reactions Nanoparticles Plant resources Pd57 G. jasminoides Pd58 Pd62 Pd66 Pd68 Pd69 Pd70 Pd71 Pd72 Au81 Ag215 AgPd248 AuPd250 AuPd251 AuPd253 AuAg258 Pt339 Ag340 Au341 Au342 Au343 Au344

C. lanatus A. annua P. glutinosa C. esculenta U. davidiana P. frutescens P. longum H. rhamnoides A. xylopoda A. nilotica C. platycladi C. platycladi C. platycladi E. condylocarpa S. marianum C. platycladi E. condylocarpa C. platycladi C. platycladi C. platycladi C. platycladi

Applications Hydrogenation of 4-nitrotoluene to 4-toluidine and 4methyl-cyclohexylamine Catalyst for Suzuki coupling reactions Synthesis of di(indolyl)indolin-2-ones dye Catalyst for Suzuki coupling reactions Catalyst for Suzuki-Miyaura cross-coupling reactions Catalysts for [3 + 2] cycloaddition reactions Catalysts for synthesis of pyrazolylphosphonate derivatives Catalyst for Sonogashira coupling reactions Catalyst for Suzuki-Miyaura coupling reactions Catalyst for alkyne/aldehyde/amine A3-type coupling Reduction of benzyl chloride to toluene Hydrogenation of 1,3-butadiene to butane Oxidation of benzyl alcohol to benzaldehyde Oxidation of benzyl alcohol to benzaldehyde Catalyst for Suzuki and Heck coupling reactions Electrocatalyst for methanol oxidation Hydrogenation of cinnamaldehyde to cinnamyl alcohol Synthesis of N-monosubstituted ureas Epoxidation of propylene to propylene oxide Epoxidation of propylene to propylene oxide Epoxidation of styrene to styrene oxide Oxidation of benzyl alcohol to benzaldehyde 32


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1

4.4. Miscellaneous Applications. Various studies have demonstrated that plant mediated noble

2

metallic nanoparticles have a broad range of applications in different domains as mentioned in

3

Table 9. Ankamwar et al., (2005) has suggested the applicability of phyto-synthesized Au-NPs

4

for chemical vapor sensing.98 Biosynthesized nanoparticles based optical sensor is also utilized

5

for the detection of metallic ions in water.225 Emmanuel et al., (2014) has demonstrated

6

electrochemical detection ability of Au-NPs modified electrode towards trace level detection of a

7

hazardous pollutant (nitrobenzene) in water samples.135 There has been increasing interest in

8

using biosynthesized nanoparticles as an active substrate for SERS techniques, for various

9

analytical and medical applications.251,252

10

Table 9. Plant mediated nanoparticles for miscellaneous applications Nanoparticles Pt53 Au76 Au78

Plant resources O. sanctum S. aromaticum A. sativum

Ag and Au80 Au98 Au114 Au123 Au133 Au135

R. damascena T. indicus A. marmelos M. longifolia S. barbata V. californica

Au136 Au137 Au and Ag147 Ag173 Ag224

A. nilotica C. zeylanicum E. officinalis C. album P. hysterophorus A. comosus C. platycladi

Ag225 AuPd251,252

Applications Water electrolysis Enhance the response of the colorimetric urea biosensor SERS substrate inside human fetal lung fibroblast HFL-1 cells Modified glassy carbon electrode Vapor sensing Detection of thiamine Efficiency in absorbing infrared radiation Direct electrochemistry of 4-NP SERS activity for detection of 2-aminothiophenol and crystal violet Trace level detection of hazardous pollutant nitrobenzene SERS substrate for molecular sensing Phase transfer and transmetallation SERS activity with rhodamine 6G Photoluminescence Detection of zinc and copper ions in water SERS activity with rhodamine 6G

11

33



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1

5. LIMITATIONS AND CHALLENGES

2

Though, there are numerous benefits of plant mediated synthesis of noble metallic nanoparticles,

3

there is still a lot of obstacles to be addressed. One significant constraint of plant mediated

4

synthesis is the complex and diverse nature of phytochemicals present in plant systems. So,

5

identification and purification of individual phytoconstituents from complex biomass and

6

determination of their role in bioreduction reactions as well as in controlling size, morphology

7

and the crystal structure of nanoparticles under a given set of reaction condition is still a

8

challenging task. So, for elucidation of exact mechanism of bioreduction reaction using plant

9

extract needs more experimentation.

10

Attaining high reproducibility, maximizing homogeneity and scaling-up of nanoparticles

11

production are key challenging factors for the biosynthesis of metallic nanoparticles using plants.

12

Plant systems are exposed to a variety of environmental, incidental and intentional exposures.

13

Various primary and secondary metabolites are therefore up- or down-regulated for the survival

14

of the plants in the changing environment, which ultimately influence the reproducibility of plant

15

materials for fabrication of nanoparticles. High polydispersity is another most critical concern to

16

be considered for the biosynthesized nanoparticles to improve their performance in various

17

domains. Varying phytochemical composition of plant extracts is determining factor for this

18

issue. Industrial-scale production of plant mediated nanoparticles for various commercial

19

applications is also a most important challenging concern. Low abundance of raw materials,

20

variable molecular composition of various phytochemicals and the heterogeneity of plant

21

extracts are key responsible factors for these issues.

34


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1

Use of plant tissue culture technique, homogenization of the plant’s secondary metabolites

2

profile, use of automated synthesis reactors, isolation, purification and identification of a

3

particular bioreducing fraction are probably the few steps to go forward for attaining

4

reproducibility, homogeneity and large scale production of biocompatible metal nanoparticles

5

using various plant resources. By applying these techniques, large scale production of

6

homogeneous and commercially viable nanoparticles can be achieved. To get more control over

7

morphology, monodispersity and stability of nanoparticles, genetically engineered plant

8

resources with optimized phytochemical composition, can also be utilized.

9

As far as commercial applications of the plant mediated nanoparticles is concerned, well-

10

characterized nanoparticles should be used for the best results. Plant mediated nanoparticles are

11

generally characterized so far only for size, shape and over all composition. However, various

12

other properties like agglomeration/aggregation, purity, surface area, surface chemistry and

13

surface charge are scantly reported in literature for plant mediated nanoparticles. These

14

properties are required to be characterized well before applying biosynthesized nanoparticles in

15

various domains. These properties are identified by the U.S. Environmental Protection Agency

16

for nanomaterial characterization and suggested their importance for defining their applications,

17

associated toxicities and environmental fate. Toxicity profiles and environmental impacts study

18

of biogenic nanoparticles are also important aspects to be considered. Despite numerous

19

developments in the field of nanobiotechnology, the assessment of toxic effects of biofabricated

20

nanoparticles on environment and public health are still not explored well. Therefore, evaluation

21

of toxicity profile and environmental effects of these nanoparticles as compared to chemically-

22

grown nanoparticles are also need to be considered. The synthesis of nanomaterials using eco35



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Page 36 of 87

1

friendly and biocompatible biological extracts could lower the toxicity of the resulting

2

nanomaterials up to some extent. However, more systematic research is still required to define

3

complete eco and human toxicity profile of biofabricated nanoparticles, particularly if

4

nanoparticles intended for in-vivo applications. One approach to avoiding such toxicity concerns

5

is to use only well-characterized and benevolent plant extracts with low or nil toxicity profile.

6

In recent years many researchers have therefore tried to establish a stable system for

7

fabrication nanoparticles with significant homogeneity in terms of morphology and size. In

8

addition to this, adsorption of bioorganics of plant extracts on the surface of nanoparticles is

9

assumed to be the reason responsible for nanoparticles stabilization. This irreversible binding of

10

the bioorganics of the plant extract may hinder the subsequent functionalization of the

11

nanoparticles with other ligands and limit their use for various specific applications. In order to

12

explore the plant systems to its highest potential, it is crucial to know the biochemical and

13

molecular mechanism of nanoparticles synthesis. The plant systems are not fully explored;

14

therefore, there are many opportunities for budding researchers to explore the plant systems for

15

synthesis of commercially valuable metallic nanoparticles. For commercial purposes, it is

16

beneficial to have a combined experimental study involving the tools of biotechnology,

17

nanotechnology, bioprocess engineering, chemical engineering, genetic engineering and plant

18

physiology for the detail spectrum investigation of biosynthesized nanoparticles. The stability of

19

biofabricated nanoparticles is another important aspect to be considered. It is very important to

20

ensure the stability of nanoparticles upon years of storage. It is important that nanoparticles

21

remain stable without any significant change of morphology, shape, size and structure. More

22

studies are also required to evaluate the long term stability of biofabricated nanoparticles. 36


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1

SUPPORTING INFORMATION

2

Table no. S1-S7 represented the details characteristics of plant mediated noble metal

3

nanoparticles. This material is available free of charge via the Internet at http://pubs.acs.org.

4

Table S1. Living plants or plant biomass mediated synthesis of metallic nanoparticles

5

Table S2. Plant extract mediated synthesis of Pt-NPs

6

Table S3. Plant extract mediated synthesis of Pd-NPs

7

Table S4. Plant extract mediated synthesis of Au-NPs

8

Table S5. Plant extract mediated synthesis of Ag-NPs

9

Table S6. Phytochemical mediated synthesis of metallic nanoparticles

10

Table S7. Plant mediated synthesis of bimetallic nanoparticles

11 12 13

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Graphical abstract

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Noble Metal Nanoparticles: Plant-Mediated Synthesis, Mechanistic

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