Sensors and Actuators B 151 (2010) 6570

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Sensors and Actuators B: Chemical

journal homepage: www.elsevier.com/locate/snb

A novel sensitive nonenzymatic glucose sensor based on perovskite

LaNi0.5 Ti0.5 O3 -modied carbon paste electrode
Yulong Wang a , Yanhong Xu b , Liqiang Luo a , Yaping Ding a,b, , Xiaojuan Liu a , Anquan Huang a
a
b

College of Sciences, Shanghai University, Shanghai 200444, PR China

Shanghai Key Laboratory of Modern Metallurgy & Materials Processing, School of Materials Science and Engineering, Shanghai University, Shanghai 200444, PR China

a r t i c l e

i n f o

Article history:
Received 28 July 2010
Received in revised form
20 September 2010
Accepted 21 September 2010
Available online 29 September 2010
Keywords:
Nonenzymatic sensor
Glucose
Perovskite
Amperometry

a b s t r a c t
A novel sensitive nonenzymatic glucose sensor was reported based on perovskite LaNi0.5 Ti0.5 O3 (LNT)
modied carbon paste electrode (CPE). The surface characterization of the modied electrode and the
bare CPE was examined by scanning electron microscopy (SEM). The high electrochemical activity of LNT
to electrocatalytic oxidation of glucose in alkaline medium was characterized by cyclic voltammetry and
amperometry, and the experimental conditions such as the amount of LNT, the concentration of NaOH
and the applied potential were investigated in detail. The glucose sensor was applied to the quantication
of glucose with a high sensitivity of 1630.57 A mM1 cm2 and a low limit of detection of 0.07 M. The
novel glucose sensor also exhibited good reproducibility, long-term stability, as well as high selectivity
with no interference from common interfering substances such as ascorbic acid, dopamine and uric acid.

1. Introduction
Diabetes mellitus is a chronic but treatable disease affecting
about 200 million people around the world [1], and the development of various sensors for fast and reliable monitoring of glucose
for the treatment and control of diabetes has been a focal subject in analytical chemistry for a few decades [2]. Optical methods
have been commonly used for the indirect detection of glucose
[36]. Besides, electrochemical methods have been one of the subjects of considerable interest [710] because a low detection limit
and high sensitivity can be achieved easily. Most of the electrochemical methods are based on the use of the glucose oxidase
that specically catalyzes the oxidation of glucose to gluconic
acid and H2 O2 , and introduce mediators which enable the reduction of H2 O2 at low potentials causing about change of current.
Accordingly, the concentration of glucose can be determined by
way of monitoring the change of current response [11]. However, the most serious problem of the enzymatic sensor is lack
of stability due to the intrinsic nature of enzyme, the activity of
which can be easily affected by temperature, pH, humidity, and
toxic chemicals [12], so the nonenzymatic electrochemical glucose sensors [13] have attracted considerable attention in recent

Corresponding author at: Department of Chemistry, College of Sciences, Shanghai University, Shangda Road No. 99, Shanghai 200444, PR China.
Tel.: +86 21 66134734; fax: +86 21 66132797.
E-mail address: wdingyp@sina.com (Y. Ding).
0925-4005/$ see front matter 2010 Elsevier B.V. All rights reserved.
doi:10.1016/j.snb.2010.09.052

2010 Elsevier B.V. All rights reserved.

few years. A variety of enzyme-free electrochemical glucose sensor

based on different material modied electrodes have been reported
[1417], for example Ni/Al layered double hydroxide nanosheet
lm on Ti substrate [14], PtPb nanowire array electrode [16],
etc.
Perovskite mixed oxides as the inorganic material have been
widely investigated and applied in the areas of electrochemical gas
sensors [18], solid fuel cells [19] and lots of oxidation and reduction
catalytic processes due to their photocatalytic property [20], magnetic properties [21], electrically active structure [22] and dielectric
property [23]. In our previous study, a series of perovskite-type
composite oxides LaNi0.5 Ti0.5 O3 (LNT) and LaNi0.5 Ti0.5 O3 NiFe2 O4
were synthesized by solgel method and used to immobilize the
glucose oxidase as a novel material in the phosphate buffer solution
[24]. In the further research, we are amazed that the electrocatalytic activity of LNT toward glucose oxidation is more excellent
in alkaline solution. The results showed that LNT revealed high
electrocatalytic activity and excellent stability for glucose determination, which has been utilized as the basis of the fabrication of
a nonenzymatic sensor for electrochemical detection of glucose.
To the best of our knowledge, this is the rst time that a perovskite material LNT modied carbon paste electrode (CPE) was
employed in the development of nonenzymatic amperometric glucose sensors. The prepared sensor was applied to detect blood
serum samples and the result demonstrated that the application
of a LNT modied electrode was feasible in glucose detection indicating a breakthrough in nonenzymatic sensors using perovskite
materials.

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Y. Wang et al. / Sensors and Actuators B 151 (2010) 6570

2. Experimental
2.1. Apparatus and reagents
All electrochemical experiments were carried out on CHI 842B
electrochemical workstation (Shanghai Chenhua Co. Ltd., China).
A conventional three-electrode system was adopted. The working
electrode was a perovskite LNT modied CPE, the counter electrode
was a Pt wire and the reference electrode was a saturated calomel
electrode (SCE). All potential values given below were referred to
the SCE. The surface of the bare CPE and the modied electrode
were characterized using scanning electron microscopy (SEM, JSM6700F, 15.0 kV).
LNT was prepared according to our previous report [24]. -dGlucose, graphite powder (spectral reagent), parafn oil, NaOH,
HNO3 , and C2 H5 OH were purchased from the Sinopharm Group
Chemical Reagent Co., Ltd., Shanghai, China. All reagents were of
analytical reagent grade. All solutions were prepared with double
distilled water. NaOH (0.1 M) solution was chosen as the supporting
electrolyte.

2.2. Fabrication of LNT modied CPE

Graphite powder and parafn oil were mixed at the ratio of
3:1 (w/w) in the agate mortar for 20 min. The mixture was rmly
packed into the glass tube (i.d. = 3.0 mm) which had been ultrasonicated in HNO3 , NaOH solution and double distilled water in turns,
and then the copper wire was inserted from another end of the
tube. The CPE was polished with a piece of weighing paper and
rinsed thoroughly with double distilled water.
3 mg perovskite material LNT was dispersed in 1 mL double
distilled water, and then the suspension was ultrasonicated for
over 2 h. After that, 10 L of the homogeneous suspension was
spread evenly onto the well-polished CPE surface with a syringe
and allowed to be dried by infrared lamp for 20 min to build
a LNT modied CPE. The electrode was washed by double distilled water and stored at room temperature when it was not
used.

Fig. 1. SEM images of the bare CPE (A) and LNT modied CPE (B).

3.2. Electrocatalytic oxidation of glucose at LNT modied

electrode

3. Results and discussion

In order to test the electrocatalytic activity of the LNT modied CPE, the cyclic voltammograms were obtained at bare and LNT
modied CPE in 0.1 M NaOH solution without and with glucose,
respectively (Fig. 2). Fig. 2A exhibits no pair of redox peaks on
the bare CPE in the potential range from 0.1 to 1.1 V (curve a) in
0.1 M NaOH solution and the oxidation of glucose starts at approximately 0.9 V (curve b). In contrast, the LNT modied CPE shows one
couple of redox peaks with oxidation peak at 0.48 V and the corresponding reduction peak at 0.33 V in blank NaOH solution, which
are assigned to the Ni(III)/(II) redox couple forming in the alkaline medium [25] (Fig. 2B, curve a). Upon the addition of glucose,
there is a great enhancement of the oxidation peak current (curve
b) at more negative potential 0.5 V, indicating enhanced electrocatalytic properties of perovskite LNT modied CPE. According to
the literatures [2527], the oxidation of glucose to glucolactone
(two hydrogen are liberated in this process) can be catalyzed by
the Ni(III)/(II) redox couple in the alkaline medium and the electrooxidation mechanism was given by the following reactions which
has been used as the basis of the fabrication of a nonenzymatic
sensor for electrochemical detection of glucose:

3.1. Characterization of LNT modied electrode

LNTNi(II) + OH
LNT(OH )Ni(III) + e
sol

(1)

LNT(OH )Ni(III) + glucose LNTNi(II) + glucolactone

(2)

2.3. Procedure of glucose measurement

The electrochemical behavior of the modied electrode was
investigated by cyclic voltammetry (CV) in a 0.1 M NaOH solution
at different scan rates. The LNT modied CPE was evaluated as a
nonenzymatic glucose sensor in 0.1 M NaOH solution at desired
potential. Amperometric curves were obtained after adding a glucose solution of certain concentration into the electrolyte under the
stirring conditions. The current in each experiment was recorded
after it reached the steady state.

Fig. 1 shows the surface images of the bare CPE (A) and LNT modied CPE (B), respectively by SEM. It can be seen that irregularly
shaped akes of graphite are isolated on the CPE (Fig. 1A). However, a more uniform surface appears without separated graphite
layer on the modied CPE (Fig. 1B) indicating that perovskite LNT
particles have been rmly modied on the surface of CPE. It can
also be seen that the unique faviform distribution of the LNT particles on the electrode supports high specic surface area for the
procedure of glucose measurement.

Fig. 3A shows the cyclic voltammograms of the LNT modied

CPE recorded in 0.1 M NaOH solution with 0.2 mM glucose at different scan rates. It is found that both oxidation and reduction
peak currents increase clearly with increasing scan rate. The inset
shows that the oxidation and reduction peak currents increase linearly with the square root of the scan rate, suggesting that the
electrocatalytic oxidation of glucose on the LNT modied CPE is a
diffusion-controlled process. Stability for the LNT modied CPE was

Y. Wang et al. / Sensors and Actuators B 151 (2010) 6570

150

67

0.8

0.6

100

0.4

I / mA

I / A

b
a

50

I / mA

0.6
0.4

0.2

0.0

0.2
5

10

15

20

scan rate1/2 / (mV/s)1/2

0.0
0

-0.2

0.0

0.2

0.4

0.6

0.8

1.0

1.2

-0.4

E/V

0.1

0.2

0.3

0.4

0.5

0.6

0.7

E/V

400
0.4

200

I / mA

I / A

0.2

0.0
-200
0.1

0.2

0.3

0.4

0.5

0.6

0.7

E/V
Fig. 2. Cyclic voltammograms obtained at bare CPE (A) and the LNT modied CPE
(B) in 0.1 M NaOH without (a) and with (b) glucose.

also examined by recording its 50 consecutive CV curves in NaOH

solution at a scan rate of 100 mV s1 , and results are given in Fig. 3B.
No obvious peak current change is found during 50 consecutive CV
curves, implying that the LaNi0.5 Ti0.5 O3 was rmly modied onto
the surface of CPE.
3.3. Optimization of glucose sensor performance
In order to further enhance the performance of the analytical
system for glucose sensor, the experimental conditions including
the amount of LNT, applied potential and the concentration of NaOH
solution were investigated.
In the present work, the effects of LNT amount and applied
potential on the amperometric detection of glucose were investigated by measuring current response of 20 M glucose in 0.1 M
NaOH solution (Fig. 4A). The amount of LNT was changed during the range of 15 mg mL1 (curve a) at the applied potential of
0.55 V and it can be seen that the current response increases with
the increasing amount of LNT from 1 to 3 mg mL1 and decreases
above 3 mg mL1 . The reason for this is that an increase in the
amount of redundant LNT decreased the electroconductivity and
increased the noise owing to the semiconductive nature of perovskite. So the amount of LNT 3 mg mL1 was chosen for applied
potential optimization. The working electrode was operated at different potentials between 0.4 and 0.7 V, and the result shows that
the oxidation current of glucose increases with the increase of the
potentials from 0.4 to 0.55 V, then decreases signicantly after that
(curve b). Taking the sensitivity and the signal/noise ratio into consideration, 0.55 V was chosen as the optimum applied potential.
It is well known that an alkaline medium is required for enhancing the electrocatalytic activity of the transition metal and its oxide
for oxidation of carbohydrate compounds [28]. Therefore, we also
studied the effect of hydroxide concentration on the performance of

0.1

0.2

0.3

0.4

0.5

0.6

0.7

E/V
Fig. 3. Cyclic voltammograms of the modied electrode recorded (A) in 0.1 M NaOH
solution with 0.2 mM glucose at different scan rates (inner to outer): 20, 40, 60,
80, 100, 150, 200, 250, 300, 350, 400, 450 and 500 mV/s, and 50 consecutive cyclic
voltammograms of the modied electrode in 0.1 M NaOH solution at 100 mV/s (B).
Inset: peak current as a function of square roots of different scan rate.

the sensor over the different hydroxide concentrations of 0.001 M,

0.01 M, 0.05 M, 0.1 M, 0.2 M and 0.5 M with amperometry and the
result is shown in Fig. 4B, from which it can be seen that no response
current of the oxidation of 20 M glucose is acquired in the 0.001 M
NaOH solution because of the low concentration of electrolyte.
When the concentration of NaOH increases, the current increases
obviously, because glucose is easily oxidized at high pH. However,
the high background noise is seen when the concentration of NaOH
increases above 0.1 M which is consistent with the reported experimental phenomena that an increased background current was
observed at a high NaOH concentration [25]. Therefore, 0.1 M NaOH
solution, 3 mg mL1 LNT and 0.55 V applied potential were chosen
as the optimum conditions to demonstrate the applicability of this
biosensor to the sensitive detection of glucose.
3.4. Amperometric response of glucose and calibration curve
Under optimum conditions, the typical currenttime plot upon
the successive addition of different concentrations of glucose solution is shown in Fig. 5A. When glucose was added into the NaOH
(0.1 M) solution, the current varied steeply to reach a stable value
and the modied electrode achieved 95% of the steady-state current
within 8 s. The analytical performance of glucose on the LNT modied CPE in 0.1 M NaOH solution with the applied potential of 0.55 V
is shown in Fig. 5B. There are two linear regions of glucose concentration, respectively in 0.220 M (inset, correlation coefcient,
0.9992) and in 201000 M (correlation coefcient, 0.9954) and
the respective linear equations: I (A) = 0.00905 + 0.1152C (M)

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Y. Wang et al. / Sensors and Actuators B 151 (2010) 6570

Amount of LNT / mg mL-1

0

4.5

2.5

1 M

20

I / A

I / A

100M

25

2.0

0.5 M

0.2 M

20M

4.0

15

10

10M
3.5

200

1.5

400

Time / s

5
1.0
400
0.4

0.5

0.6

800

1200

1600

Time / s

0.7

Applied Potential / V

B 100

B
40

0.2 M

60

I / A

30

0.1 M

20

2.5
2.0

40
I / A

I / A

80

0.5 M

0.05 M

20

10

0.0

0.001 M

100

150

1.0
0.5

0.01 M

1.5

0
200

10

15

20

Cglucose / M

time / s

500

1000

1500

2000

2500

Cglucose / M

Fig. 4. (A) Effect of the amount of LNT (a) and the applied potential (b) on glucose
(20 M) detection in 0.1 M NaOH solution. (B) Amperometric responses of the LNT
modied CPE at 0.55 V applied potential upon successive additions of 20 L 1 mM
glucose into 10 mL NaOH solution with different concentrations of 0.001 M, 0.01 M,
0.05 M, 0.1 M, 0.2 M and 0.5 M. The detection solution was continuously stirred.

and I (A) = 3.031 + 0.05328C (M). Here this phenomenon of the

two linear regions may be due to the adsorption of intermediates
[29]. The limit of detection (LOD) is 0.07 M (S/N = 3) and the sensitivities are 1630.57 and 754.14 A mM1 cm2 which are much
higher than those reported in enzymeless glucose sensor [30,31].
Comparisons to other nonenzymatic glucose sensing methods and
materials are made and given in Table 1. Comparisons are focused
on nonenzymatic electrochemical glucose sensors based on different kinds of materials. As it can be seen from Table 1, the proposed
glucose sensor shows good sensing performance in terms of LOD
and sensitivity. Compared with other materials, the advantage of
this electrode material is obvious. For example, compared with

Fig. 5. (A) Currenttime response obtained in 0.1 M NaOH solution by increasing different concentrations of glucose on the modied electrode at 0.55 V. Inset:
currenttime response of the low concentration of glucose. (B) Calibration curve of
glucose concentration on the modied electrode.

Ni/AlLDH nanosheet lm directly on Ti foil [14], we can see the

proposed electrode exhibits higher sensitivity.
3.5. Interferences and blood serum sample measurement
One of the most important analytical factors for an amperometric biosensor is the ability of the sensor to discriminate the
interfering species having electroactivities similar to the target analyte. The easy oxidizable compounds such as ascorbic acid (AA),
dopamine (DA) and uric acid (UA) are normally co-existed with
glucose in natural samples. Because the normal physiological level
of glucose in the human blood is about 30 times of AA, DA and UA

Table 1
Comparison of various nonenzymatic glucose sensors based on different materials.
Sensitivity (A mM1 cm2 )

Glucose sensors

Applied potential (V)

Ni/AlLDH lm on Ti foil
PtPb nanowire array electrode

0.7
0.2
0.45

24.45
11.25
10.81

0.65

251.38

0.6
0.55
0.1
0.25
0.55

371.43
202
16
32
1630.57
754.14

Ordered mesoporous carbon modied electrode

Cu nanocluster/multiwall carbon nanotube
modied glassy carbon electrode
CuO nanorods modied the graphite substrates
Nanoscale nickel hydroxide modied CILE
Porous gold electrode
Perovskite LaNi0.5 Ti0.5 O3 modied CPE

Linear range
5 M to 10 mM
011 mM
0.52.5 mM
2.55 mM
0.73.5 mM
4 M to 8 mM
50 M to 23 mM
020 mM
0.220 M
20 M to 1 mM

LOD (M)

Ref.

8
20

[14]
[16]
[29]

0.21

[32]

4
6
2
6
0.07

[33]
[34]
[35]
This work

Y. Wang et al. / Sensors and Actuators B 151 (2010) 6570

69

value after 40 days, reecting the good stability of the nonenzymatic glucose sensor.

25
20

I / A

8 M UA

8 M AA

4. Conclusion

8 MDA

15
10
5
200 M glucose

100

200

t/s
Fig. 6. Amperometric response of glucose (200 M) in the absence and presence of
8 M AA, DA and UA at the LaNi0.5 Ti0.5 O3 modied CPE at an applied potential of
0.55 V in 0.1 M NaOH solution.

[36], we studied the interference effect of 8 M AA, DA and UA on

the amperometric response of 200 M glucose in the present work.
At this level, the current response for such electroactive interfering
species to that of glucose by the sensor was below 5% at an applied
potential of 0.55 V in 0.1 M NaOH solution (seen in Fig. 6). In addition, inuences of maltose and fructose on the glucose detection
were also examined and the results showed that the addition of
50 M maltose and 100 M fructose did not have any effect on the
determination of 200 M glucose. Therefore, good selectivity can
be obtained with the prepared sensor.
In order to see if there is no matrix effect in blood, the prepared sensor was applied to determine blood serum samples with
amperometric method. Amperometric detection was carried out
at the applied potential of 0.55 V in 10 mL 0.1 M NaOH solution
under stirring conditions with 10 L blood serum injected and
the nal concentration was diluted to 120 M which is in the
linear range of the proposed sensor and can be detected sensitively. The quantitative determination of blood serum samples was
carried out using the standard addition method and the results
are shown in Table 2 which were obtained as mean from three
determinations. The detected results of the blood serum samples
are in agreement with those determined by hospital and recovery values in the range of 95.6101.9 (5%) in Table 2 indicate
that the proposed method is reliable for the determination of glucose and has the potential for practical applications in real human
serum.
3.6. Reproducibility and stability of the nonenzymatic sensor
The reproducibility and stability of the nonenzymatic glucose
sensor were evaluated via the comparison of the currents of different electrodes. The amperometric response of three LNT modied
CPEs to 0.1 mM glucose was tested independently, and the relative standard deviation (RSD) was 4.43%. A reproducible current
response with a RSD of 3.96% was observed for 5 successive assays
of 0.1 mM glucose. The long-term stability was explored by measuring a glucose solution intermittently, and the electrode was stored
at room temperature when it is not in use. The result shows that
the catalytic current response maintains more than 90% of its initial
Table 2
Determination of glucose in human blood serum samples.
Serum samples

Hospital
(mM)

Sensor
(mM)

RSD
(%)

Added
(mM)

Recovery
(%)

1
2
3

3.3
2.6
3.1

3.45
2.83
3.20

3.2
6
2.2

5
5
5

95.6
101.6
101.9

In this work, a novel nonenzymatic glucose sensor based on perovskite LNT modied CPE was fabricated without any adhesive. LNT
modied CPE showed high electrocatalytic activity for the glucose
electrooxidation. A lower detection limit and the high sensitivity
were obtained compared with those previously reported, and good
linear dependence of the amperometric response of the modied
electrode on the glucose concentration was achieved. In addition,
the interference from the oxidation of common interfering species
such as AA, DA and UA can be avoided for the blood serum samples
detection. Therefore, the perovskite material LNT holds the promise
for the development of nonenzymatic glucose sensor.
Acknowledgments
This research is supported by the National Natural Science
Foundation of China (No. 20975066), the Nano-Foundation of Science and Techniques Commission of Shanghai Municipality (No.
0952nm01500), Leading Academic Discipline Project of Shanghai
Municipal Education Commission (J50102), the Ph.D. Innovation
Foundation of Shanghai University (No. SHUCX091030).
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Biographies
Yulong Wang received the BS degree from Hebei University, Hebei, China, in 2008.
She is currently studying for a MS degree at the Department of Chemistry, Shanghai
University, Shanghai, China. Her current research interest involves the electrochemical sensors based on chemically modied electrode.
Yanhong Xu is an engineer of chemistry in China. She received her BS degree from
China University Mining and Technology, China, in 1994 and MS degree from Beijing
University of Chemical Technology, China, in 2004. She is now studying for her PhD
degree in School of Materials Science and Engineering in Shanghai University. She
engages in nano-structured materials research: preparation, characterization and
application.
Liqiang Luo is an associate professor of analytical chemistry in Shanghai University.
He received his BS and MS degree from Henan Normal University, China, in 1994 and
1997, respectively; and PhD degree from Changchun Institute of Applied Chemistry,
Chinese Academy of Sciences, China, in 2000. His research interests involve modied
electrode and biosensors.
Yaping Ding is a professor of analytical chemistry in Shanghai University. She
received her PhD degree in analytical chemistry from the University of Science and
Technology of China in 2003. Her research interests involves in the electroanalytical
chemistry, the nano-analytical chemistry and the chemometrics.
Xiaojuan Liu received the BS degree from Anhui Normal University, Anhui, China,
in 2008. She is currently studying for a MS degree at the Department of Chemistry,
Shanghai University, Shanghai, China. Her current research interest involves the
biosensor.
Anquan Huang received the BS degree from Shanghai Television University, Shanghai, China. He works in the Campus Hospital, Shanghai University. His current
research interest is internal medicine.