Physica E 44 (2011) 97104

Contents lists available at ScienceDirect

Physica E
journal homepage: www.elsevier.com/locate/physe

Green synthesis of silver and gold nanoparticles using Rosa damascena and its
primary application in electrochemistry
Sayed M. Ghoreishi n, Mohsen Behpour, Maryam Khayatkashani
Department of Analytical Chemistry, Faculty of Chemistry, University of Kashan, Kashan 87317-51167, Islamic Republic of Iran

a r t i c l e i n f o

abstract

Article history:
Received 30 June 2011
Received in revised form
24 July 2011
Accepted 28 July 2011
Available online 4 August 2011

Biosynthesis and characterizations of nanoparticles have become an important branch of nanotechnology. In this paper, green synthesis of gold nanoparticles (AuNPs) and silver nanoparticles (AgNPs) using
the ower extract of Rosa damascena as a reducing and stabilizing agent, has been discussed. This
approach is simple, cost-effective and stable for a long time, reproducible at room temperature and in
an eco-friendly manner to obtain a self-assembly of AuNPs and AgNPs. The resulting nanoparticles are
characterized using UVvis, TEM, XRD and FT-IR spectroscopic techniques. A modied glassy carbon
electrode using AuNPs (AuNPs/GCE) was investigated by means of cyclic voltammetry in a solution of
0.1 M KCl and 5.0  10  3 M [Fe(CN)6]3  /4  . The results show that electronic transmission rate between
the modied electrode and [Fe(CN)6]3  /4  increased.
& 2011 Elsevier B.V. All rights reserved.

1. Introduction
The metal nanoparticles have been synthesized using a variety
of methods, including chemical and physical methods. Although
most of the methods may successfully produce pure and welldened nanoparticles, these methods are quite expensive and
potentially dangerous to the environment. Use of biological
organisms such as microorganisms and plant extracts could be
an alternative to chemical and physical methods in an ecofriendly manner and green synthesis [13].
Plant extracts may provide a better alternative to nanoparticle
production. Several plants have been studied for biosynthesis of
nanoparticles. The extracts of Aloe vera [4], Papaya [5], Lemongrass
[6], Cinnamommum camphora [7], Neem [8], Tamarind [9], Emblica
ofcinalis [10], Clove [11] and Syzygium aromaticum [12] have
shown potential in reducing Au3 ions to form gold nanoparticles
(Au) and silver nitrate (Ag ) to form silver nanoparticles (Ag).
However, Brassica juncea germinating seeds [13] have been used
for AgAuCu alloy nanoparticle synthesis. Recently, Philip et al.
demonstrated green synthesis of gold and silver nanoparticles
using Hibiscus rosa sinensis [14], Murraya Koenigii leaf-assisted
[15], Mangifera indica [16] and Krishna tulsi [17]. Dubey et al.
studied the synthesis and characterizations of silver and gold
nanoparticles using leaf extract of Rosa rugosa [18] and Tanacetum
vulgare (tansy) [19].
The genus Rosa includes 200 species and more than 18,000
cultivars [20]. Despite the large number of cultivated rose

Corresponding author. Tel.: 98 3615912395; fax: 98 3615912930.

E-mail address: s.m.ghoreishi@kashanu.ac.ir (S.M. Ghoreishi).

1386-9477/$ - see front matter & 2011 Elsevier B.V. All rights reserved.
doi:10.1016/j.physe.2011.07.008

varieties, the main rose producers in the world obtain from

R. damascena. R. damascena (Rosaceae) (Fig. 1) is a widely cultivated ornamental plant. Several therapeutic effects including
anti-inammatory, astringent, expectorant, laxative, cardiac tonic
and aperients have been described for the ower extract of
R. damascena. Roses also have an economic importance for their
ower as a source of natural fragrances and avorings [21]. Four
avanoids, quercetin, quercitrin, rutin and luteolin [22] and two
polyphenols, gallic acid and myricetin (Fig. 2) [23] were detected
and quantied in fresh owers of R. damascena. The owers
contain an essential oil with citronellol, nerol, geraniol and
beta-phenylethanol. Flavanoids and polyphenols naturally occur
in the plant kingdom and generally present in fruits, vegetables,
leaves, nuts, seeds, owers and barks [24]. Quercetin mainly
occurs in plants as glycosides, such as rutin and quercitrin. Over
the past years, avanoids have gained tremendous interest
because of their protective effects on DNA damage [25], antiinammatory [26] and their free radical scavenging activities
[27], that can protect against cardiovascular diseases [28] and
certain kinds of cancers [29].
Herbs and minerals are the integral parts of traditional
medicine in many countries. In traditional Iranian medicine, by
adding R. damascena extract to pure gold, they obtained a red
powder (this red powder is called Kushta Tila). After processing
the R. damascena extract using gold, a drug with cardiotonic and
nervine tonic properties can be formulated [30].
We can presume that the avanoids, polyphenolic and essential
oil, which are abundant in R. damascena appear to be responsible
for accelerated reduction and capping of AuNPs and AgNPs.
Essential oil is poorly water soluble and hence may not be among
prime moieties involved in the reduction and capping process.

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S.M. Ghoreishi et al. / Physica E 44 (2011) 97104

reducing agents, reversing oxidation by donating electrons and

hydrogen ions. We can presume that the avanoids and polyphenols, which are abundant in R. damascena extract show
characteristic absorption peaks and appear to be responsible for
accelerated reduction and capping of R. damascena extract. Other
compounds of R. damascena are poorly water soluble and hence
may not be among prime moieties involved in the reduction
process. Gold colloidal nanoparticles were used to realize a
modied GCE and enhance electronic transmission rate between
the electrode and [Fe(CN)6]3  /4  .

2. Experimental
2.1. Materials
Chloroauric acid (HAuCl4  3H2O) and silver nitrate (AgNO3)
were obtained from Merck and used as received. A stock solution
containing 1  10  3 M HAuCl4  3H2O and 1  10  2 M AgNO3
were prepared in deionised water. All other reagents were of
analytical grade. R. damascena ower collected from Kashan, Iran,
was cleaned thoroughly with deionised water and dried at 303 K.
Then 10 g of R. damascena ower was passed through a sieve
(30 mesh) and stirred with 100 mL deionised water at 300 K for
5 min and ltered to get the extract.

Fig. 1. Photograph of R. damascena used in the biosynthesis.

OH
OH
OH

OH O

2.2. Apparatus

Luteolin: R = H
Quercetin: R = OH
Quercitrin: R = Rhamnopyranosyl

Rutin: R = Rutinoside

OH
OH
OH

OH

OH
OH

OH
OH

HO
OH

Myricetin

Gallic acid

Fig. 2. Flavanoids and polyphenols content in R. damascena extract.

However, we restricted our attention to avanoids and polyphenols compounds due to its high antioxidant capacity. Natural
avanoids have been shown to serve as a reductant for the
enlargement of Au nanoparticles [31] and the synthesis of Ag
nanoparticles in reverse micelles [32], and thus there is a possibility that it may be responsible for the formation and growth of
AuNPs and AgNPs. Thus, this oxidized form of avanoids and
polyphenols may dictate the growth and capping of the AuNPs
and AgNPs. It was understood that avanoids also prevent agglomeration and stabilize the AuNPs in an aqueous solution [33].
In the present study, we rst report the synthesis of AuNPs and
AgNPs by the reduction of gold and silver ions using R. damascena.
R. damascena extract contains antioxidant compounds and act as

The FT-IR spectra were recorded by a Perkin-Elmer FT-IR

spectrophotometer. X-ray diffraction (XRD) measurements were
recorded using Rigaku D-max C III, X-ray diffractometer using
UVvis spectroscopy
Ni-ltered Cu Ka radiation (l 1.5406 A).
measurements were carried out on Perkin-Elmer spectrophotometer operated at a resolution of 1 nm. TEM samples of the AuNPs
and AgNPs synthesized using the R. damascena extract were
prepared by placing drops of the reaction mixture over carbon
coated copper grids and allowing the solvent to evaporate. TEM
images were obtained on a Philips EM208 transmission electron
microscope with an accelerating voltage of 100 kV. Voltammetric
measurements were carried out using an Autolab potentiostat/
galvanostat PGSTAT 35 (Eco chemie Utrecht, Netherlands) equipped
with GPES 4.9 software. The electrochemical cell was equipped
with a glassy carbon electrode (GCE) as the working, a platinum
electrode as the counter and an Ag/AgCl electrode as the reference
electrode. All experiments were carried out at room temperature.
2.3. Synthesis of AuNPs and AgNPs
15 mL R. damascena ower extract was added to a vigorously
stirred 30 mL aqueous solution of HAuCl4 (1  10  3 M) and
stirred continuously for 2 min and the nal volume was adjusted
to 50 mL with deionised water at room temperature. In a typical
reaction procedure, 10 mL of R. damascena ower extract was
added to 30 mL of AgNO3 (1  10  2 M) solution and the nal
volume was adjusted to 50 mL with deionised water. The resulting solution became brown in color after 5 min. Color intensity
increases with the increase in HAuCl4  3H2O and AgNO3 concentrations at a xed volume fraction of extract.
2.4. Assembling of AuNPs modied glassy carbon electrode
The bare glassy carbon electrode (bare-GCE) was polished into
a mirror-like surface with 0.5 and 0.05 mm alpha Al2O3 and then
rinsed ultrasonically with water baths, so that any physically
adsorbed species is removed. The cleaned glassy carbon electrode
was modied by dip coating, using immersion times (2 h) in the

S.M. Ghoreishi et al. / Physica E 44 (2011) 97104

colloidal nanoparticles solutions. The modied electrode was

electrochemically characterized by cyclic voltammetry (CV) in a
0.1 M KCl solution that contains 5.0  10  3 M [Fe(CN)6]3  /4  .

3. Results and discussion

3.1. UVvis absorbance spectroscopy
UVvis spectroscopy is an important technique to ascertain
the formation and stability of nanoparticles in aqueous solution.
Spectral analysis for the development of nanoparticles at different reaction conditions was observed using UVvis spectral
analysis. The reaction mixtures developed an array of colors
after 2 min for AuNPs and 5 min for AgNPs of incubation under

different conditions indicating the synthesis of a variety of

AuNPs and AgNPs. The UVvis spectra of the reaction mixtures
are also shown in Figs. 3 and 4. AuNPs and AgNPs gave sharp
peak in the range of visible region of the spectrum. Fig. 3a and b
shows the effect of varying R. damascena concentrations on
AuNPs and AgNPs synthesis. With an increase in R. damascena
extract from 9 to 15 mL for AuNPs and 5 to 10 mL for AgNPs,
consistently an increase in peak absorbance was found in UVvis
spectrum. However, visual inspection of the solutions revealed
color changes from light pink to deep red for AuNPs and dark
yellow to brown for AgNPs with an increase of R. damascena
quantity in each reaction solution. It is well known that AuNPs
and AgNPs exhibit lovely pink-ruby red and brown colors, and
these colors arise due to excitation of surface plasmon vibrations. The AuNPs and AgNPs surface plasmon band occurs in the

2.5

3.0

2.0

2.0

f
e
d

1.5

3 months

1.5

10 day
2 months

Absorbance

2.5

Absorbance

99

24 h

1.0

1.0
a
0.5

0.5

0.0
480

0.0
400

450

500

550
600
650
Wavelength (nm)

700

750

680

2.0

2.0

f
e

1.5

1.5

d
c
b

1.0

10 day
2 months

Absorbance

Absorbance

580
Wavelength (nm)

3 months

1.0

24 h

0.5

0.5

0.0
380

430

480
530
580
Wavelength (nm)

630

680

Fig. 3. (a) UVvis absorption spectrum of AuNPs at different R. damascena extracts

quantity (30 mL HAuCl4 1  10  3 M with 9, 10, 11, 12, 13, 14 and 15 mL
R. damascena extract). (b) UVvis absorption spectrum of AgNPs at different
R. damascena extracts quantity (30 mL AgNO3 1  102 M with 5, 6, 7, 8, 9 and
10 mL R. damascena extract).

0.0
380

480
Wavelength (nm)

580

Fig. 4. (a) UVvis absorption spectrum of AuNPs recorded as a function of reaction

time with R. damascena extracts (30 mL HAuCl4 1  10  3 M with 15 mL
R. damascena extract). (b) UVvis absorption spectrum of AgNPs recorded as a
function of reaction time with R. damascena extracts (30 mL AgNO3 1  10  2 M
with 10 mL R. damascena extract).

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S.M. Ghoreishi et al. / Physica E 44 (2011) 97104

range of 510550 nm and 400450 nm in an aqueous medium,

respectively. UVvis spectra of these aliquots were monitored as
a function of time of reaction (Fig. 4a and b). These biosynthesized AuNPs and AgNPs were laid aside at room temperature
3 months later. There is no obvious aggregation in the solution,
and its absorption value shows only a little reduction. The
results from Fig. 4a and b suggest that the AuNPs and AgNPs
synthesized by R. damascena have very good stability.
3.2. TEM analysis of nanoparticles
The particle size can be determined theoretically using techniques like UVvis spectroscopy, XRD and experimentally using
microscopic techniques like TEM. The morphology of the synthesized AuNPs and AgNPs was also determined by TEM images.
AuNPs and AgNPs to be conned within a supporting matrix, likely
comprised biomolecules acting as a capping agent or stabilizer
during synthesis, and thus controlling nanoparticle growth and

clustering. Alternatively, it is possible that the biomolecules present in the R. damascena extract were believed to be the agents
responsible for reducing the Au3 and Ag to Au1 and Ag1. TEM
images of the AuNPs and AgNPs obtained under normal conditions
demonstrate that nanoparticles were self-assembled, with average
sizes ranging from 10 to 30 nm, as shown in Fig. 5. Fig. 5(ad)
shows typical TEM micrographs of AuNPs and AgNPs synthesized
after reduction of HAuCl4 and AgNO3 with R. damascena extract.
Interpretation of TEM images of AuNPs at 15 and 10 mL and AgNPs
at 10 and 5 mL of R. damascena suggests an increase in particle size
with a decrease in extract quantity. As the amount of R. damascena
extract in the reaction medium is increased, the average edge
lengths of the AuNPs and AgNPs decrease. From the above discussions, for the formation of AuNPs and AgNPs, synthesized in
various ratios of HAuCl4 and AgNO3 with R. damascena extract, it
can be said that the size of these nanoparticles are highly affected
by the ratio of HAuCl4 and AgNO3 versus R. damascena extract.
The rate of formation of AuNPs and AgNPs was found to be slower

Fig. 5. TEM micrographs of AuNPs and AgNPs synthesized at (a) 30 mL HAuCl4 1  10  3 M with 15 mL R. damascena extract, (b) 30 mL HAuCl4 1  10  3 M with 10 mL
R. damascena extract, (c) 30 mL AgNO3 1  10  2 M with 10 mL R. damascena extract and (d) 30 mL AgNO3 1  10  2 M with 5 mL R. damascena extract.

S.M. Ghoreishi et al. / Physica E 44 (2011) 97104

According to the equation [34]

25

Distribution percentage (%)

kl
b cos y

where L is the particle size (nm), k is the Scherrer constant, b is

the full width half maximum, y is half of Bragg angle and l is the
wavelength of X-ray [35]. Fig. 7a and b shows a representative
XRD pattern of the AuNPs and AgNPs synthesized by the
R. damascena compound after completion of the reduction.

20

15

3.4. FT-IR studies

10

0
9

10 11 12 13 14 15 16 17 18 19 20 21 22
Particle Diameter (nm)

35
30
Distribution percentage (%)

101

25

Typical FT-IR absorption spectra of R. damascena extract before

and after bioreduction are shown in Fig. 8. FT-IR spectra were
carried out to identify the potential biomolecules R. damascena
responsible for the reduction and capping of the bioreduced AuNPs
and AgNPs. A number of broad bands are observed in the region
9003500 cm  1 centered at 3440, 1740, 1620 and 1370 cm  1.
R. damascena have been reported to consist of avanoids and
polyphenols which form the major component [22,23]. The IR bands
observed at 1370 and 1740 in R. damascena extract are characteristic
of the CO and CQO stretching modes of the carbonyl functional
group in ketones, aldehydes and carboxylic acids. The peak at
1620 cm  1 can be assigned to the vibrational modes of CQC
double bonds of these molecules. The proposed oxidized structure
of avanoids, gallic acid and myricetin are shown in Fig. 9. The
carbonyl groups from the avanoid and polyphenolic compound
have a stronger ability to bind Au and Ag ion, so that the avanoid

20
15
10
5
0
8

10

11

12

13

14

15

16

17

18

19

Particle Diameter (nm)

Fig. 6. (a) Histogram of the size distribution of AuNPs synthesized by treating
15 mL R. damascena extract with 30 mL HAuCl4 1  10  3 M solution.
(b) Histogram of the size distribution of AgNPs synthesized by treating 10 mL
R. damascena extract with 30 mL AgNO3 1  10  2 M solution.

at the lowest concentration and hence absorbance is also weaker.

The obtained histogram using the enlarged TEM graphs revealed
that almost 32% of the AuNPs were 16 nm and 23% of the AgNPs
were 21 nm in diameter (Fig. 6a and b). In AuNPs and AgNPs the
particles are almost quasi-spherical with mean size of 15.3 nm and
18.3 nm, respectively.
3.3. XRD analysis of nanoparticles
The crystalline nature of AuNPs and AgNPs was further
conrmed from X-ray diffraction (XRD) analysis. This was compared to the particle sizes determined by TEM images. For XRD
the particles were calculated using the DebyeScherrer equation.
The average crystallite size according to DebyeScherrer equation
calculated using the width of the (1 1 1) peak is found to be 14 nm
for AuNPs and 19 nm for AgNPs nearly in agreement with the
particle size obtained from the TEM image of AuNPs and AgNPs.

Fig. 7. (a) XRD patterns of AuNPs synthesized by treating 30 mL HAuCl4

1  10  3 M with 15 mL R. damascena extract. (b) XRD patterns of AgNPs synthesized by treating 30 mL AgNO3 1  10  2 M with 10 mL R. damascena extract.

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S.M. Ghoreishi et al. / Physica E 44 (2011) 97104

groups of the avanoid and polyphenol and the hydroxyl groups are
oxidized to carbonyl groups.

and polyphenolic compound could form a coat over the metal

nanoparticle to prevent gathering of particles. The linkages between
carbonyl groups and metal ion give a well-known signature in the
FT-IR spectrum. After the bioreduction of R. damascena extract with
Au3 and Ag , the shift in the peak at 1740 cm  1 is attributed to
the binding of carbonyl group with nanoparticles. Also, the hydroxyl
peak at 3440 cm  1 decreases in the presence of nanoparticles,
which indicates Au3 and Ag ions are reduced with the hydroxyl

3.5. Assembling of AuNPs modied glassy carbon electrode

Electrocatalytic activity of biosynthesized AuNPs was measured by cyclic voltammetry (CV). Fig. 10 shows the CV responses
of 5.0  10  3 M [Fe(CN)6]3  /4  in a 0.1 M KCl solution at the
bare-GCE and AuNPs assembled electrodes. The electron transfer
kinetics of a redox couple in the solution on the AuNPs assembled
electrodes depend on the surface of the GCE. As can be seen,
Fe(CN)36  /4  shows a couple of well-dened redox waves at bareGCE electrode (Fig. 10, curve c) with a peak-to-peak separation of
190 mV at 45 mV s  1 scan rate. After the self-assembly of AuNPs,
an obvious increase in redox peak currents and decrease in peakto-peak separation are observed (Fig. 10, curve d). An increase in
current responses and decrease in DEp on the AuNPs assembled
GCE electrodes were attributed to rapid electron transfer rate on
the GCE surface. On the other hand, the self-assembled AuNPs
were successfully assembled on the GCE electrode and acted as
the inert electron and mass transfer blocking layer. The typical
cyclic voltammograms of the AuNPs assemble GCE in 0.1 M KCl
solution that contains 5.0  10  3 M [Fe(CN)6]3  /4  with scan
rates of 25, 45, 65, 85, 105, 125 and 145 mV s  1 as shown in
Fig. 11. As can be observed, the oxidation peak potential shifted
with increasing the scan rates toward a more positive potential,
conrming the kinetic limitation of the electrochemical reaction.
In the range of 25145 mV s  1, the anodic peak current (Ipa) of
5.0  10  3 M [Fe(CN)6]3  /4  increased linearly with an increase
in the square-root of the scan rate (u1/2). This result indicated that
the oxidation was controlled by diffusion (Fig. 11b). According to

(c)
(b)

(a)

400

900

1400

2400

1900

2900

3400

3900

Wavenumber (cm-1)
Fig. 8. FT-IR spectra of (a) dried R. damascena extract; dried powder of (b) AuNPs
and (c) AgNPs.

OH

O
OH

OH

O
OH

OH

+ 2H+ + 2eR

OH

OH

OH
OH

OH

OH

OH

+ 2H+ + 2eOH

OH

OH

OH

HO

HO

+ 2H+ + 2eOH

OH
OH

O
OH

Fig. 9. Mechanism of oxidation of avanoids, myricetin and gallic acid.

S.M. Ghoreishi et al. / Physica E 44 (2011) 97104

versus scan rate (Fig. 11a) the surface coverage of AuNPs/GCE is

5.3  10  6 mol cm  2 for n 1.

60
d

40

4. Conclusion

I / A

20

b
a

-20

-40

-60
-0.4

103

-0.2

0.2

0.4

0.8

0.6

E / V vs Ag/AgCl
Fig. 10. Cyclic voltammograms at 50 mV s  1 for the bare-GCE electrode in the
absence (curve a) and presence (curve c) of 5.0  10  3 M [Fe(CN)6]3  /4  in a 0.1 M
KCl solution; the AuNPs assembled GCE in the absence (curve b) and presence
(curve d) of 5.0  10  3 M [Fe(CN)6]3  /4  in a 0.1 M KCl solution.

The spanking new and simple method for biosynthesis of

AuNPs and AgNPs by R. damascena extract offers a valuable
contribution in the area of green synthesis and nanotechnology
without adding different physical and chemical steps. The synthesis of AuNPs and AgNPs by R. damascena extracts indicated that
avanoids and polyphenols compounds could be one of the key
biomolecules serving multiple roles. The nanoparticles were
characterized by UVvis, TEM, XRD and FT-IR measurements.
This synthetic green method obtained stable aqueous solutions of
AuNPs and AgNPs. This simple, low cost, non-toxic and ecofriendly method for development of AuNPs and AgNPs may be
valuable in environmental, biotechnological, pharmaceutical and
medical applications. Moreover, this system could also be used in
electrochemical applications. The biosynthesized AuNPs are
assembled to the surface of the GCE and could raise electronic
transmission rate between the electrode and [Fe(CN)6]3  /4  .
Acknowledgments
The authors wish to express their gratitude to the University of
Kashan for supporting this work.

60
50
40

References

30
I / A

20
10
0
-10
-20
-30
-40
-50
-0.6

-0.2

0.2

0.6
1.0
E / V vs Ag/AgCl

1.4

1.8

Fig. 11. Cyclic voltammograms of AuNPs assembled GCE in 5.0  103 M

[Fe(CN)6]3  /4  in a 0.1 M KCl with scan rates of 25, 45, 65, 85, 105, 125 and
145 mV s  1. (a) Plot of peak current versus scan rate, (v/mV s  1). (b) Plot of peak
current versus the square-root of scan rate, (v/mV s  1)1/2.

RandlesSevcik equation [36]

Ip 2:69  105 n3=2 AD1=2 Cu1=2

where n is the number of electrons transferred in the reaction, u is

the scan rate, A is the surface of the electrode, C is the concentration of reactant and Ip is the peak current of the reactant. Linear
regression equations were as follows:
Ipa mA 0:1363u1=2 mV s1 1=2 22:501,

R2 0:991

An approximate estimate of the surface coverage of the

electrode was made by adopting the method used by Sharp
[37]. According to this method, the peak current is related to
the surface concentration of mediator, ! , by the following
equation:
Ip n2 F 2 A! n=4RT

where n represents the number of electrons involved in the

reaction, A is the surface area (0.0314 cm2) of the GCE, !
(mol cm  2) is the surface coverage of mediator and other symbols
have their usual meanings. From the slope of anodic peak currents

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