Food Anal.
Methods
DOI 10.1007/s12161-011-9214-4
Determination of Melamine by Differential Pulse
Polarography/Application to Milk and Milk Powder
Ümmihan T. Yilmaz & Zehra Yazar
Received: 6 December 2010 / Accepted: 10 February 2011
# Springer Science+Business Media, LLC 2011
Abstract Melamine made headlines in September 2008
because it was found to be the contaminant responsible for
the deaths of several infants and making many more sick.
Determination of trace melamine is very important. Therefore,
in this work a novel, sensitive and reliable method was
developed using differential pulse polarography. The most
suitable buffer system was found to be Britton–Robinson
(B–R) buffer, pH 11.2. The melamine peak in this medium
appeared at about −50 mV, it responded well to standard
additions and high reproducibility was obtained. The
calibration graph was linear in the concentration range of
melamine from 1.0 to 66.4 μM with a correlation coefficient
of 0.999. The limit of detection (LOD) and limit of
quantification (LOQ) were obtained as 0.3 and 1.0 μM,
respectively. The current was characterized as being
adsorption-controlled process. The proposed method was
successfully applied to the determination of melamine in
spiked milk and milk powder. The linear dynamic ranges
observed for melamine concentration in milk and milk
powder samples were between 1–58 and 10–57 μM,
respectively. The sufficiently good recoveries and low
standard deviations for the data reflect the high accuracy
and precision of proposed differential pulse polarographic
method.
Keywords Determination . Differential pulse
polarography . Melamine . Milk . Milk powder
Ü. T. Yilmaz (*) : Z. Yazar
Science and Letters Faculty, Department of Chemistry,
Nevşehir University,
50300 Nevsehir, Turkey
e-mail: ummihan@nevsehir.edu.tr
Introduction
Melamine (2,4,6-triamino-1,3,5-triazine) is normally used
in the manufacture of melamine-formaldehyde resins for
surface coatings, laminates, and adhesives and in the
production of flame retardants (Chang 1994). Melamine
became a topic of much discussion in early 2007, when
veterinary scientists determined it to be the cause of
hundreds of pet deaths due to pet food contamination
(Brown et al. 2007; Filigenzi et al. 2008). The melamine-
tainted milk powder incident in China led to serious
concerns about food safety. The main toxic effects of
exposure to melamine are formation of bladder stones and
hyperplasia in the urinary bladder (International Agency for
Research on Cancer; Baynes et al. 2008). The primary
target organ for melamine toxicity is the kidney. There is
uncertainty with respect to the time scale for the develop-
ment of kidney damage. Thus, the U.S. Food and Drug
Administration (FDA) applied a tolerable daily intake
(TDI) of 0.5 mg/kg in body weight considering possible
health effects which might occur with repeated consump-
tion of melamine contaminated products over a relatively
short period (FDA). The FDA describes the risk to
human health associated with eating products from
animals that have been fed with melamine. Consequently,
there has been growing concern about the significance
and toxicity of melamine; this fact encouraged the
development of methods for its trace determination in
various sample materials.
For the determination of melamine, some methods such
as gas chromatography/mass spectrometry (GC/MS) (Xu
et al. 2009; Li et al. 2009; Miao et al. 2009; Ibánez et al.
2009; Zhao et al. 2010), high-performance liquid chroma-
tography (HPLC)/MS (Xia et al. 2009; Muñiz-Valencia
et al. 2008; Filigenzi et al. 2007), capillary zone electro-

phoresis/MS (CE/MS or UV) (Karaseva et al. 2003; Meng
et al. 2009; Klampfl et al. 2009; Wen et al. 2010),
potentiometry (Liang et al. 2009) and some electrochemical
methods (Cao et al. 2009, 2010; Tsung-Hsuan et al. 2010)
have been proposed.
A coupled capillary column system was developed for the
quantitative determination of melamine with isotope internal
standard in dairy products using GC/MS without derivatiza-
tion (Xu et al. 2009). The detection limit was 0.01 mg kg−1.
Melamine in fresh milk was extracted by zirconia hollow
fiber, enriched on zirconia coating of the hollow fiber; then it
was analyzed using GC-MS. The detection limit was
0.001 μg/mL (Li et al. 2009). Melamine in egg was
determined using liquid chromatography (LC)-MS/MS and
UPLC Ultra-Performance Liquid Chromatography-MS/MS.
The limits of detection (LODs) were 10 and 5.0 μg kg−1,
respectively (Xia et al. 2009).
Melamine in milk powder samples was determined using
CZE with either UV or MS. The developed CZE method
allowed the determination of melamine in milk powder down
to a level of 0.50 mg/kg using UV detection and 0.25 mg/kg
when ESI quadrupole/TOF MS Time of Flight Mass
Spectrometry was employed for detection (Klampfl et al.
2009). A polymeric membrane ion-selective electrode for
determination of melamine was prepared. The membrane
electrode showed near-Nernstian response (54 mV/decade)
to the concentration range of 5.0×10−6 to 1.0×10−2 mol l−1.
The potentiometric sensor has been applied in the determi-
nation of melamine in milk samples (Liang et al. 2009).
Melamine was determined using the oligonucleotide
modified gold electrodes. The electrochemical probe of
ferricyanide was used to investigate the interactions
between oligonucleotides and melamine. The detection
limit was 9.6×10−9 M (Cao et al. 2009). Electrochemical
sensor was developed for melamine using 3,4-dihydrox-
yphenylacetic acid. The electrochemical behavior of
3,4-dihydroxyphenylacetic acid in the presence of mela-
mine was studied. The anodic peak currents of 3,4-
dihydroxyphenylacetic acid obtained by differential pulse
voltammetry are linear with the logarithm of melamine
concentrations in the range from 1.0×10−8 to 5.0×10−6 M
with a linear coefficiency of 0.997. The detection limit is
3.0×10−9 M (Cao et al. 2010). Determination of melamine
has been developed by employing oxidized polycrystalline
gold electrode (poly GE). Poly GE successfully showed the
peak for melamine adsorption at 1.1 V, purely based on the
detection of adsorption signals of melamine at the poly GE
surface. The proposed poly GE successfully detected the
melamine signal (0.5–6.7 μM) in tainted milk powder
samples (Tsung-Hsuan et al. 2010).
Some of these methods are usually difficult because they
involve time-consuming and tedious pre-concentration tech-
niques such as ion exchange, solvent extraction or hydride
Food Anal. Methods
generation to lower the risks of interference problems. Losses
of elements are also possible and high of costs instruments
limit the application of current methods.
Polarographic methods, using dropping mercury electrodes
(DMEs), offer useful alternatives since they allow faster,
cheaper and safer analysis (Somer and Dogan 2008; Inam and
Cicek 2009; Sarigul and Inam 2009). Validation can be made
by working with different electrolytes and at different pH
values. There is no need for long and tedious electrode
preparation procedures after each usage. The results obtained
with differential pulse polarography (DPP) are very repro-
ducible because with the use of DME the behavior of the
electrode is independent of its past history.
From a review of the literature, the methodology for the
determination of melamine using DPP has not yet been
described. The purpose of this work is to examine the
polarographic determination of melamine, find out the
optimum analysis conditions and apply the method for the
determination of melamine in various media, i.e., milk and
milk powder. Also, electrochemical behaviors of melamine
are investigated with cyclic voltammetry (CV).
Experimental
Apparatus
A BAS model (Bioanalytical Systems, Epsilon Basic Plus
Potentiostat/Galvanostat, USA) electrochemical analyzer
was used for DPP and CV measurements. A three-
electrode system was used, consisting of a platinum counter
electrode, an Ag/AgCl (3 M NaCl) reference electrode and
a DME as a working electrode. pH values were measured
with a WTW pH/ION 735 (WTW Instruments, Germany)
pH meter.
Reagent
Melamine, analytical grade, was purchased from Sigma
(USA). Stock solution was prepared in ethanol–water
(50:200, v/v) at a concentration of 0.01 M and was stored
in a refrigerator. Working standard solutions were prepared
by dilution of stock solution with water. All chemicals (i.e.,
electrolyte, solvents and other reagents) used were of
analytical-reagent grade (proanalysis). Triply distilled water
was used in the preparation of all solutions. Solutions of
10−3 M and more dilute ones were prepared before use in
order to avoid the aging process of solution.
The mercury used in the DME was obtained from Merck
(Darmstadt, Germany). Contaminated mercury was cleaned
by passing it successively through dilute HNO3 (3.0 M) and
water columns in the form of fine droplets by using a
platinum sieve. The collected mercury was dried between
Food Anal. Methods
sheets of filter paper. Before use, a DPP polarogram of this
mercury was recorded in order to confirm the absence of
impurities.
Britton–Robinson (B–R) buffer solution was prepared in
such a way that 2.3 mL of glacial acetic acid, 2.7 mL of
phosphoric acid (85%) and 2.47 g of boric acid dissolved
by dilution with water to 1.0 l; 50-mL portions of this
solution were taken, and the pH was adjusted by the
addition of an appropriate amount of 2.0 M NaOH to the
desired value.
Analytical Procedure
Ten milliliters (10 mL) of supporting electrolyte solution of
HClO4, HCl, acetate, phosphate, ammonia or B–R buffer was
placed in the polarographic cell and de-oxygenated with high-
purity nitrogen (99.999) for about 5 min. Background
polarograms were obtained by scanning the potential from
0.0 V to about −1,400 to −2,200 mV (vs. Ag/AgCl)
depending on the pH of the solution. Next, the polarographic
responses of 1×10−5 to 1×10−3 M melamine at the DME
were analyzed in various electrolyte solutions. Analytical
curves for melamine were obtained by standard addition of
melamine. The linear concentration range was between 1.0
and 66.4 μM. Optimum conditions for the analytical
determination of melamine using DPP were found as follows:
pH=11.2 B–R buffer electrolyte, peak potential of −50 mV,
scan rate of 5 mV s−1, a pulse amplitude of 50 mV.
Procedure for Analysis of Spiked Milk and Milk Powder
Samples
The utility of the proposed method was proven by melamine
spiked milk and milk powder samples with melamine. For
this purpose, 1.0 mL of milk sample was spiked with 1.0 mL
1×10−2 M melamine solution in 8.0 mL acetonitrile, which
removes milk proteins more effectively. The same proce-
dure was also followed in parallel for melamine-free milk
sample. After homogenizing the samples for 20 min, they
were centrifuged for 20 min at 9,000 rpm (6,758.32×g
units) to remove the milk protein residues. From the
supernatant, 0.1 mL of melamine-free aliquots were
collected, transferred to the polarographic cell containing
9.9 mL of B–R buffer solutions at pH 11.2 supporting
electrolyte solutions. Differential pulse polarogram was
recorded, and the milk sample that contains 1×10−3 M
melamine was added two times. We added 0.1 mL of
spiked melamine sample to the polarographic cell contain-
ing 9.9 mL electrolyte and 0.1 mL of melamine-free
aliquots. In the polarography cell, the concentration of
melamine in milk sample is 1.0×10−5 M.
Next, 0.5 g of the milk powder sample was spiked in
1.0 m 1× 10−2 M melamine solution and then 9.0 mL of
acetonitrile solution was added. The mixture was vor-
texed for 1 min and then centrifuged for 20 min at
9,000 rpm (6,758.32 × g units) to remove the serum
protein residues, after which the supernatant was dis-
carded. After the completion the above procedure for milk
powder, 0.1-mL aliquots then added to the cell containing
9.9 mL of B–R buffer solution at pH 11.2. Differential
pulse polarograms were recorded and melamine determi-
nation in melamine-spiked milk powder was performed
from the peak current at about −65 mV using melamine
standard additions.
Results and Discussion
Effect of pH and Buffer Solution
The DP polarograms of melamine were taken in 0.1 M HClO4,
in 0.1 M HCl, pH 1–6, 12 acetate electrolyte, pH 11, 12.5
phosphate buffer, pH 7, 10 ammonia buffer and pH 2–13 B–
R buffer. The peak of melamine was not observed in the
acidic solution (Table 1a). The polarographic currents of
melamine obtained in the phosphate and ammonia buffer
were very weak (Table 1a). The B–R buffer was chosen for its
wide pH range applicability. For the basic study of the
electrochemical behavior of cyanuric acid, differential pulse
polarographic responses were examined over the pH range of
2.0–13.0. Based on the results, peak of melamine was not
observed until pH 10.5. Figure 1a shows typical DPP
polarograms of 20 μM melamine within the pH range of
10.5–12.7 (Table 1b). As shown in Fig. 1a, the peak potential
of melamine at the DME was found to be pH-dependent and
shifted to more negative values as pH values increased.
Figure 1b shows the peak currents for melamine depending
on the pH of the buffer solution. As shown, the peak current
of melamine increased in the pH range 10.5–11.2, decreased
strongly at pH values greater than 11.2 and there was no
peak at pH 13. In spite of this the maximum peaks
current were obtained at pH 11.2 for melamine. As a
result, optimum conditions for analytical determination of
the melamine by DPP were as follows: pH 11.2 B–R
buffers, at a reduction potential of −50 mV, 2 s drop
time, 50 mV pulse amplitude.
Linear Range and Detection Limit
The peak current–potential curve is the most useful
analytical signal for DPP technique. Therefore, the rela-
tionship between peak current (at about −50 mV) and
concentration was studied by DPP using optimum con-
ditions. The consecutive additions of melamine onto the
pH 11.2 B–R buffer gave a linear relationship between the
peak currents and concentrations (Fig. 2). The calibration
 Food Anal. Methods

Table 1 Polarographic behav-

ior of melamine in various Ion Electrolyte Epeak (mV) I (nA) Peak shape C (M)
electrolytes
a. Polarographic behavior of melamine in various electrolytes
Melamine pH=11.0 phosphate −35 264 Sharp 2×10−5
−136 120 Broad
pH=12.4 phosphate −188 316 Broad
−257 461 Sharp
pH=7.0 NH3-NH4+ −40 200 Broad
−150 115 Sharp
pH=10 NH3-NH4+ No peak No peak No peak
pH=4.0 HAc-NaAc No peak No peak No peak 2×10−4
pH=12.0 HAc-NaAc −288 70 Broad 1×10−2
0,01 M HClO4 No peak No peak No peak 5×10−4
0.1 M HCl No peak No peak No peak
b. Polarographic behavior of melamine Britton–Robinson buffer electrolytes
Melamine pH=10.5 −10 700 Sharp 2×10−5
−64 120 Broad
pH=11.2 −50 829 Sharp
−107 230 Broad
pH=11.7 −85,6 574 Sharp
−148 237 Broad
pH=12.4 −165 331 Broad
−223 320 Sharp
pH=12.7 −182 213 Broad
−234 249 Sharp

graph was in the range of 1.0–66.4 μM with the linear
regression equations given by


Ip ðmAÞ ¼ 0:036C ðmMÞ  0:021 R2 ¼ 0:999 ðn ¼ 10Þ
LOD and LOQ were obtained as 0.3 and 1.0 μM,
respectively, according to the relation k × Sb/b (Currie
1999) (where k=3 for LOD and k=10 for LOQ, and Sb is
the standard deviation of the current measured for the blank

Fig. 2 DPP responses for several concentrations of melamine: a

Fig. 1 a Differential pulse polarograms of 20 μM melamine in
pH 10.5–12.7 B–R buffer solution. b Dependence of pH on the DPP
peak currents of 20 μM melamine
10.0 mL pH 11.2 B–R buffer solution; b a+0.1 mL 1×10−3 M
melamine; c b+0.1 mL 1×10−3 M melamine; d c+0.1 mL 1×10−3 M
melamine; e d+0.1 mL 1×10−3 M melamine; f e+0.1 mL 1×10−3 M
melamine; g f+0.1 mL 1×10−3 M melamine; hg+0.1 mL 1×10−3 M
melamine
Food Anal. Methods

solution containing 0.3 μM melamine and b is the slope of Table 3 Influence of interfering species on the recovery of 10 μM
melamine
the calibration curve). The straight line has a slope of
0.036 μA/μM, an intercept of 0.021 μA and a correlation Interfering C Recoveries Interfering C Recoveries (%) of
coefficient of 0.999. The high sensitivity of DPP is species (μM) (%) of species (μM) melamine
accompanied by very good repeatability. This analytical melamine
performance was evaluated from five repeated measure- Pb2+ 100 98.9 Al3+ 100 97.3
ments of electrochemical signal of 10.0 μM melamine
Ni2+ 98.6 K+ 97.8
solution for the supporting electrolyte was 4.8% (Table 2).
Cd2+ 97.8 Ba2+ 95.3
These values confirmed the sensitivity of the proposed
Fe3+ 95.0 Mg2+ 99.8
method for the determination of melamine.
Zn2+ 90.0 Ca2+ 96.9
Se4+ 98.9 NO3− 97.8
Interference Studies
Co2+ 97,9 SO42− 99.8
Cu2+ 95.8 Cl− 95.8
The selectivity of the proposed method for melamine was
Mn2+ 94.7 Se4+ 98.9
investigated in the presence of some inorganic ions found
mostly in milk (Yaman and Cokol 2004; Inam and Somer
2000) and milk powder (Martins et al. 2002). The
interference studies were performed using the various Al(III), K(I), Ba(II), Na(I), Ca(II), Mg(II), NO3−, SO42−,
interfering ions, most of which are electro-active [e.g., Cu Cl and I− are polarographically inactive species and
−

(II), Fe(III), Co(II), Ni(II), Pb(II), Zn(II), Cd(II), Mn(II), Se
(IV)] and some are inactive [e.g., Al(III), K(I), Ba(II), Na
(I), Ca(II), Mg(II), NO3−, SO42−, Cl−]. The degree of
interference effects was treated as the recoveries of
10 μM melamine in the presence of 10 times larger
concentration of interfering ions (Table 2). Under the
optimum conditions for polarographic determination
10 μM melamine, Cu (−182 mV), Fe (−1,440 mV), Cd
(−660 mV) and Zn (−1,351 mV) appeared at a more
negative potential than melamine (−50 mV). Thus, the
polarographic peaks of these ions did not overlap the
melamine peak, and therefore they had no significant effect
on the polarogram of melamine. Since added ions did not
cause a change in peak height of melamine, determination
of melamine was made with standard additions (Table 3).
Co, Ni, Hg, Mn, Pb and Se(IV) did not seriously affect the
melamine peak, because there was no peak response for
these cations at the studied pH and concentrations.
therefore had no serious effect on the determination of
melamine. The results obtained in the presence of interfer-
ing ions are summarized in Table 3.
Cyclic Voltammetry
A current–potential curve for 30 μM of melamine using
pH 11.2 B–R buffers is presented in Fig. 3. The
voltammetric behavior of melamine is characterized by
one reduction peaks and one oxidation peak in this medium
at a hanging mercury drop electrode (Fig. 3). As shown in
Fig. 3, the cyclic voltammogram was recorded by the
potential scan within the potential range of 0 to −600 mV;
one cathodic peak was observed at about −307 mV and one
anodic peak occurred at about −37 mV (Fig. 3). The
separation between the anodic and cathodic peaks, ΔEp, and

Table 2 Statistical parameters for the polarographic determination of

melamine

Parameter Supporting Milk Milk powder

electrolyte

Measured potential (mV) −50 −44 −65

Linearity range (μM) 1–66 1–58 10–57
Slope (μA/μM) 0.036 0.025 0.008
Intercept (μA) 0.021 0.018 0.040
Correlation coefficient 0.999 0.998 0.996
LOD (μM) 0.3 0.3 3.3
LOQ (μM) 1.0 1.0 10
Repeatability of the peak 4.8 2.1 3.7
current (RSD%) Fig. 3 A cyclic voltammogram of 30 μM for melamine at a hanging
mercury drop electrode with scan rate 100 mV s−1
 Food Anal. Methods

the cathodic peak current, Ipc, behavior as a function of the

square root of the sweeping rate, v1/2, was studied in the
range of scan rates between 25 and 1,000 mV s−1. The
process showed the quasi-reversible (Gokce et al. 2005)
nature of the reduction peak at about −307 mV on mercury
electrode. The peak at about −307 mV is quasi-reversible
because of these criterion: Ip increases with v1/2 but do not
keep the proportionality; ΔEp is larger than 60/n mV and
increases with v; the cathodic peak potential, Epc shifts to
negative value with the increase in v. For quasi-reversible
reactions Ip is not proportional to v1/2 (Greef et al. 1985)
and the voltammograms of a quasi-reversible are more
drawn out and exhibit a large separation in peak potentials
compared to those of reversible system as was observed in
this study.
The dependence of peak current (Ip) on scan rate (ν) was
studied in the range 25–1,000 mV s−1. While a linear
relationship was observed between peak current Ip (μA)
and scan rate ν (mV/s) (Eq. 1), a linear relationship was not
observed between the peak current (Ip) and the square root
Fig. 4 Determination of spiked melamine in milk: a 9.9 mL of B–R
of the scan rate (v1/2).
buffer solution (pH=11.2)+0.1 mL melamine-free milk sample; b a+

 0.1 mL 1×10−3 M melamine in milk sample; c b+0.1 mL 1×10−3 M
Ip ðmAÞ ¼ 0:0052vðmV=sÞ þ 0:1212 R2 ¼ 0:998 ð1Þ
melamine in milk sample; d c+0.1 mL 1×10−3 M melamine; e d+
0.1 mL 1×10−3 M melamine; f e +0.1 mL 1×10−3 M melamine
A plot of the logarithm of peak currents (log Ip) versus
the logarithm of scan rate (logν) gave a straight line (Eq. 2)
with a slope of 0.846, this value being close to that dynamic ranges observed for melamine concentration in
theoretically expected (1.0) for adsorption controlled milk and milk powder samples were between 1–58 and
systems (Laviron 1980). When the product or the reactant 10–57 μM, and linear regression analysis of the data gave
is strongly adsorbed, a prepeak or a postpeak is showed in the fallowing equations:
cyclic voltammogram (Wopschall and Shain 1967). These
For milk sample; I ðmAÞ ¼ 0:025C ðmMÞ  0:018ðR2 ¼ 0:998Þ
peaks are called adsorption peaks. If the adsorption is weak, For milk powder sample; I ðmAÞ ¼ 0:008C ðmMÞ  0:040ðR2 ¼ 0:996Þ
these peaks are not observed. Since adsorption peaks have
not been observed in this study, the electrode process was LOD and LOQ were calculated for milk and milk
controlled by weak adsorption (Bard and Faulkner 2001). powder (Table 2). The results confirmed the sensitivity of

 the proposed method for the detection of melamine.
log Ip ðmAÞ ¼ 0:846 logv ðmV=sÞ  1:8461 R2 ¼ 0:995 ð2Þ
The melamine determination in melamine-spiked milk
was performed from the peak current at about −44 mV
Application to Milk and Milk Powder (versus Ag/AgCl) using multiple melamine standard addi-
tions (Fig. 4). The recoveries were estimated by measuring
In order to test its application to real samples, the proposed the peak currents of extracted milk and milk powder
method was applied for the determination of melamine in samples, and comparing them with peak currents obtained
spiked milk and milk powder samples. A calibration curve after the standard additions of the same concentrations. No
was obtained for melamine in both milk and milk powder interferences were observed in a blank extracted from the
samples. Quantitative determination was possible via the milk and milk powder. Results for the recoveries of various
linear dependence of the peak height on the concentration spiked concentration are presented in Table 4. The
of melamine present in the electrolyte solution. The linear sufficiently good recoveries and low relative standard

Table 4 Determination pffiffiffiffi

of spiked melamine in milk Spiked melamine Found melamine X  ts= N a %RSD %Recovery
and milk powder samples
(in polarography cell) Milk (M) 1×10−5 0.95×10−5 (0.95±0.05)×10−5 2.1 95
a
Milk powder (M) 1×10−5 0.87×10−5 (0.87±0.08)×10−5 3.7 87
90% confidence interval (N=3)
Food Anal. Methods
(RSD) data reflect the high accuracy and precision of the
proposed differential pulse polarographic method. The high
sensitivity of the polarographic technique allows the tenfold
dilution of samples, thus avoiding matrix effects.
Conclusions
A review of the literature showed that no studies on DPP
determination of melamine have been reported so far. The
presented DPP method for the quantitative determination of
melamine was shown to be accurate and was found to be
rapid, simple and highly sensitive. The peak of melamine at
about −50 mV in pH=11.2 B–R buffer electrolyte was used
and the LOD and limit of quantification (LOQ) were
obtained as 0.3 and 1.0 μM, respectively. The obtained
results are very reproducible since, with the use of DME,
the surface of the electrode is always new and the behavior
of the electrode is independent of its past history.
The developed method was successfully applied for
determination of melamine content in melamine spiked
milk and milk powder. Calibration curves were obtained for
melamine in milk and milk powder. The relationship
between peak current (Ip) and concentration of melamine
was linear for milk and milk powder.
The main advantage of this procedure is the possibility
of determining the trace quantities of melamine directly
from natural samples (milk and milk powder) without any
previous treatment, such as extraction, clean-up and
derivatization or pre-concentration, which are tedious,
time-consuming and can lead to pollution.
Acknowledgements This work was supported by the Scientific and
Technological Research Council of Turkey (TÜBİTAK) through grant
no: 109T538.
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