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Department of Chemistry, Faculty of Mathematics and Natural Sciences Universitas Indonesia, Depok 16424,
Indonesia
Abstract. Cholesterol has a wide range of physiological function in the human body, but if the concentration
exceeds the normal limit, it can trigger diseases such as arteriosclerosis. Therefore a rapid and accurate method
of determining cholesterol is developed. Of all the methods, enzymatic sensors have received a lot of attention,
but these sensors is easily denatured. Therefore, the determination of cholesterol using non-enzymatic sensors is
widely developed. In this study, we developed electrochemical non-enzymatic cholesterol sensor using Cu/SPE,
Ni/SPE, CuNi/SPE electrode combined with FIA system at flow rate of 0.5 mL/min and KOH concentration of 1
M. Cu/SPE, Ni/SPE, and CuNi/SPE in FIA systems have LODs of 1.08, 13.59, 1.24 M and sensitivity of
3,584.97, 465.98, 3.258.54 A mM-1 cm-2 respectively. Cu/SPE, Ni/SPE, CuNi/SPE sensors have excellent
repeatability, reproducibility, and stability. Sensors are also selective against cholesterol from common
interfering substances such as glucose, sucrose, fructose, ascorbic acid, and NaCl. Cu/SPE, Ni/SPE, and
CuNi/SPE succeeded in determining cholesterol in packaging milk samples and showing 1.88%, 3.59% and
3.05% yield differentials and 99.79 %, 98.61 % and 99.02% recovery.
INTRODUCTION
EXPERIMENTAL METHOD
a b c
d e f
Figure 1. Cyclic Voltametry of composite electrode (a) Cu/SPE, (b) Ni/SPE and (c) CuNi/SPE in KOH 1M
at different cholesterol concentration (scan rate = 100 mV/s). Plot of peak current vs. concentration for (d)
Cu/SPE, (e) Ni/SPE, and (f) CuNi/SPE
The SEM EDX analysis of the CuNi/SPE composite electrode is shown in Figure 6.
From Figure 6, it appears that the Ni deposit is quite evenly distributed whereas the Cu
deposit is stacked at several points. In addition, the amount of Cu deposit is much more than
Ni because Cu is much more easily reduced than Ni. Besides Cu and Ni, there are also other
elements such as carbon (C), oxygen (O), chloride (Cl), and gold (Au). The presence of the C
atom comes from the SPE electrode material. The presence of the O atom comes from the
deposit oxidized by oxygen in the air, but the oxidation is not too large. The presence of Cl
atoms may be derived from the used distilled or comparative electrode Ag/AgCl. While Au
atoms are derived from the coating process when measuring SEM EDX because the sample is
less conductive.
Figure 2. SEM images, elemental mapping, and EDX data of CuNi/SPE composite electrodes
Figure 3 shows the amperometric current response of the Cu/SPE, Ni/SPE, and
CuNi/SPE composite electrodes to the addition of a cholesterol solution of varying
concentrations. The resulting current response is then divided by the amount of loading to see
the efficiency of the catalyst used. Figure 7 shows the higher concentration of injected
cholesterol solution giving rise to cholesterol oxidation current. Linearity, LOD, and
sensitivity for Cu/SPE, Ni/SPE, and CuNi/SPE summarized in Table 1 indicate the three
sensors have small LOD values and high sensitivity. Of the three electrodes, Cu/SPE has the
smallest LOD value and the greatest sensitivity because the amount of Cu loading in SPE is
the largest. However, when viewed from the peak per-loading ratio, Ni/SPE is the most
efficient composite electrode because its peak per-loading ratio is the largest.
a b c
Figure 3. chronoamperometry data of composite electrode (a) Cu/SPE, (b) Ni/SPE, and (c) CuNi/SPE on
cholesterol addition of 0.1 mM, 0.5 mM, 1.0 mM, 2.0 mM, 3.0 MM, 4.0 mM, 5.0 mM, and 10.0 mM of 0.1
mL in KOH 1 M at 0.5 mL/min flow rate.
Tabel 1. Linearity, LOD (Limit of Detection), dan Sensitivity
a b c
Figure 4. Chronoometerometric data of composite electrode (a) Cu/SPE, (b) Ni/SPE, and (c) CuNi/SPE on
addition of 5.0 mM cholesterol as much as 0.1 mL in KOH 1 M with a flow rate of 0.5 mL/min in the first
and second weeks
a b c
Figure 5. Chronoamperometry data of composite electrode (a) Cu / SPE, (b) Ni / SPE, and (c) CuNi / SPE
on addition of cholesterol 5.0 mM of 0.1 mL in KOH 1 M at a flow rate of 0.5 ML / min for five
consecutive days
Table 3. Average peak, standard deviation and% RSD stability
a b c
c
Figure 6. Results of selectivity test of composite electrode (a) Cu/SPE, (b) Ni/SPE, and (c) CuNi/SPE in
KOH 1 M with addition of 0.1 mL cholesterol solution 5.0 mM, glucose 5.0 MM, ascorbic acid 5.0 mM, 5.0
mM sucrose, 5.0 mM NaCl, and 5.0 mM fructose at a 0.5 mL/min flow rate
To find out how accurately the sensor is made, a recovery test is done. Prior to the
recovery test, a cholesterol spike was prepared by mixing the analytes of 5 ml standard
cholesterol solution with a sample solution with known concentration in a 100 mL flask. To
get% recovery, spike cholesterol levels are measured compared to calculated cholesterol
levels. The results summarized in Table 4 indicate that Cu/SPE, Ni/SPE, and CuNi/SPE with
FIA systems have a high accuracy of accuracy at the time of measurement.
Table 4. The results of recovery test (recovery)
CONCLUSIONS
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