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Idress and Elbashir. Current Trends Anal Bioanal Chem 2017, 1(1):50-56
Volume 1 | Issue 1
Copyright: © 2017 Idress MO, et al. This is an open-access article distributed under the terms of the Creative Commons Attribution
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Research Article Open Access
SCHOLARLY PAGES
Current Trends in
Analytical and Bioanlaytical Chemistry
• Page 50 •
*Corresponding author: Professor Abdalla A Elbashir,
Department of Chemistry, Faculty of Science, University of
Khartoum, Sudan, E-mail: aaelbashir@uofk.edu
Received: September 28, 2017: Accepted: November 14, 2017:
Published online: November 16, 2017
Citation: Idress MO, Elbashir AA (2017) Development and
Validation of Potentiometric ZnO Nanorods Modied Ion
Selective Electrode for Determination of Gemioxacin in
Pharmaceutical Formulation. Current Trends Anal Bioanal
Chem 1(1):50-56
Development and Validation of Potentiometric ZnO Nanorods
-
Malaz Osman Idress and Abdalla A Elbashir*
Department of Chemistry, Faculty of Science, University of Khartoum, Sudan
Abstract
Potentiometric method for determination of Gemioxacin (GEMI) by ion selective electrode based on ZnO nanorods
incorporation with HPβ-CD as sensing ionophore and (KTFPB) potassium tetrakis- (3,5(Triouromethyl) Phenyl Borate)
ion as anionic site (additive) in Polyvinyl Chloride (PVC) membrane, without inner reference solution was developed. e
sensor shows `nearly Nernstian response over a concentration range (0.5-10000 μM) with a slope of 33.65 mv decade-1 of
concentration with a Limit of Detection (LOD) 0.1500 μM. e electrode exhibits a fast dynamic response of 2 s for a period
of 6 months without signicant change in its characteristics with excellent stability and sensitivity toward inorganic species.
e method is accurate and precise as indicated by the mean recoveries 106.43% with RSD less than 2%. e proposed
method was successfully applied for the determination of GEMI in pharmaceutical formulations.
Keywords
Potentiometric, Ion selective electrode, Zno nanorode, GEMI, PVC membrane
Introduction
Gemioxacin Mesylate (GEMI), chemically known as
[(R, S)-7-[(4Z)-3 (aminomethyl)-4-(methoxyimino)-1-pyr-
rolidinyl]-1-cyclopropyl-6-fluoro-1,4-dihydro-4-oxo-1,
8-naphthyridin-3-carboxylic acid mesylate] Figure 1. Its
fourth generation uoroquinolone antibacterial agent hav-
ing anity towards bacterial topoisomerase IV, It has broad
spectrum of activity against gram-positive and gram-nega-
tive bacteria [1]. GEMI has shown potent activity against
other major pathogens involved in respiratory tract infec-
tions, including Haemophilus inuenza and the atypical or-
ganisms, Legionella pneumophila, Chlamydia spp, and My-
coplasma spp [2]. Furthermore, the compound has shown
potent activity against many organisms that cause urinary
tract infections. e adverse reaction prole is similar to
that of older members of this class [3]. e great bactericidal
activity of GEMI is due to the presence of 4-oxo-3-carbox-
ylic acid [4].
A number of analytical methods have been reported
for the determination of GEMI in pharmaceutical for-
mulation and biological samples. ese include High
Performance Liquid Chromatography (HPLC) [5], HPLC
coupled with Mass Spectrometry (HPLC-MS) [6], Cap-
illary electrophoresis [7], Gas Chromatography-Mass
Spectrometry (GC-MS) [8], Spectrophotometery [9],
N NN
H2N
FCOOH
N
O
OCH3
Figure 1: Chemical structure of Gemioxacin.
• Page 51 •
Citation: Idress MO, Elbashir AA (2017) Development and Validation of Potentiometric ZnO Nanorods Modied
Ion Selective Electrode for Determination of Gemioxacin in Pharmaceutical Formulation. Current Trends Anal
Bioanal Chem 1(1):50-56
SCHOLARLY PAGES
Idress and Elbashir. Current Trends Anal Bioanal Chem 2017, 1(1):50-56
in pharmaceutical formulations. Ion selective electrode
consisted of PVC, dibutyl phthalate, 2-Hydroxypro-
pyl)-β-cyclodextrin (HPβ-CD) and Potassium Tetrakis
(3,5(TriFlouromethyl)Phenyl) Borate (KTFPB) as ma-
trix, plasticizer, sensing ionophore and anionic additive,
respectively were used to develop the sensor.
Materials and Methods
Chemicals and reagent
Gemioxacin was obtained from (98%, Bayer AG,
Leverkusen Germany), HPβCD (ionophore), Potassi-
um Tetrakis (3,5(TriFlouroMethyl)Phenyl) Borate (KT-
FPB) (additive), PVC (high molecular weight), dibutyl
phthalate (a plasticizer), Zinc Acetate (ZnAc), Hexam-
ethylenetetramine (HMTA) ware purchased from sigma
Aldrich (St.Louis, USA), silver wire (0.3 mm diameter),
Na2HPO4, H3PO4, KOH, acetone, isopropanol, Tetra-
hydrofuran (THF), methanol, (all solvent with HPLC
grade), Factive tablets (320 mg GEMI per tablet) [LG life
science Ltd, Kore lisansiyla Abdilbrahim ilacsan.VeT-
ic.A.S. Maslak/Istanbul 3.5.2016, 210/86], Deionized wa-
ter.
Instrument and apparatus
pH/mv meter (PHS-3E) (China), Ag/AgCl reference
electrode (Ω metrohm.Autolab, inner and outer lling
by KCl 3 M. (Netherlands), sensitive balance, magnet-
ic hot plate, thermometer, oven, SEM (Zeiss Evo LS
10.Germany).
Seed and growth ZnO nanorods
ZnO nanorods were grown by low temperature aque-
ous chemical method [19]. A silver wire (0.3 mm) was
cut in the length of 5 cm and cleaned by acetone and iso-
propanol for 2 min in each solution followed by rinsing
with deionized water and le to dry at room tempera-
ture. e silver wire was immersed three times in a seed
solution prepared by mixing alcoholic solutions of KOH
added drop wise to heated, stirred 0.03 M of zinc acetate
the resulting solution was kept under stirring for 2 hours
at 60 °C prior dipping , the wires was le to dry at room
temperature. e ZnO was grown by suspending the
pre-coated Ag wire in aqueous solutions contains 0.025
M ZnAc with equimolar concentration of HMTA. e
beaker was placed in preheated oven at 70 °C to 5 hours.
e wires were cooled down, washed by deionized water
and le to dry over night. e ZnO nanorods were char-
acterized by SEM (Zeiss Evo LS 10, Germany) Figure 2.
Coating ZnO nanorods with Ion selective membrane
ZnO nanorods were coated by ion selective mem-
brane by mixing 33% PVC, 66% DBP plasticizer, 1.2%
HPβ-CD (ionophore), 0.4% KTFPB (ionic additive) in
Spectrouorimetry [10,11], Voltammetry [12] and Che-
miluminescence [13]. Most of these methods are com-
plicated involve derivatization procedures, requires in-
tensive instruments also it’s time and labor consuming.
Potentiometric sensors are easy to miniaturize and
provides a large dynamic range. In conventional ion se-
lective electrodes, Polyvinyl Chloride (PVC) is the most
commonly used matrix as the selective membrane [14].
e ion-selective membrane exhibits the selectivity with
which the sensing material responds to the analyte and
an electrochemical equilibrium is reached. e result-
ing potential dierence, formed between the phases, will
then be governed by the activity of this specic ion in the
two solution phases [15].
Potentiometric methods, using ion selective elec-
trodes, have found wide application [16,17] being sim-
ple analysis procedures, economical coasts, fast results ,
applicable over a wide range of concentrations, applica-
bility to various drug forms, with applicability to turbid
and colored solutions, preciseness and oering enough
selectivity towards the drug in the presence of various
pharmaceutical excipients.
Al-Mohaimeed, et al. [16] developed potentiometric
sensors using dierent such as ion-pairing agents Phos-
photungstic Acid (PTA), Phosphomolybdic Acid (PMA)
and Ammonium Reineckate Salt (ARS). e sensors
exhibit good selectivity for GEMI with respect to some
inorganic cations, amino acids and some pharmacolog-
ically related compounds [16]. Abo-talib demonstrated
PVC membrane sensors for the determination of GEMI.
e sensors are based on the use of the ion association
complexes of GEMI cation with ammonium reineckate
counter anions as ion exchange sites in the PVC matrix.
e membranes incorporate ion association complexes
of GEMI with dibutylsebathete, dioctylphthalate, nitro-
phenyl octyl ether. e proposed sensors were success-
fully applied for determination of GEMI in bulk powder,
pharmaceutical formulation, and biological uids [17].
Research on ZnO nanostructures have been fueled
by the observation that the material properties depend
not only on the composition but also on the size and
shape [18]. Recently, ZnO nanowires, nanorods and
nanotubes have gained much attraction due to their high
surface-to-volume ratio which makes them extremely
sensitive to minute surface changes. In addition, one-di-
mensional ZnO nanostructures are promising for sens-
ing due to their ease to grow vertically on almost any
substrate [18-20].
e aim of this work is to develop and validate a
simple, sensitive, rapid and miniaturized potentiomet-
ric ZnO nanorods based ion selective electrode without
inner reference solution for the determination of GEMI
• Page 52 •
Citation: Idress MO, Elbashir AA (2017) Development and Validation of Potentiometric ZnO Nanorods Modied
Ion Selective Electrode for Determination of Gemioxacin in Pharmaceutical Formulation. Current Trends Anal
Bioanal Chem 1(1):50-56
SCHOLARLY PAGES
Idress and Elbashir. Current Trends Anal Bioanal Chem 2017, 1(1):50-56
M) phosphate buer (H3PO4/Na2HPO4) [Ph = 3; 0.2 M]
and desired volume of drug stock solution and the volume
completed to mark by deionized water.
Preparation of GEMI sample solution
5 tablets of Factive (contain 320 mg GEMI per tablet)
were weighed and the average weight was determined then
it grounded into ne powder using mortar. Solution with
0.001 M was prepared by taken accurate weight of the pow-
der dissolved by 5 mL of 0.1 M NaOH and 5 mL of phos-
phate buer (H3PO4/Na2HPO4) [pH 3, 0.2 M] were added,
the volume was completed to 250 mL by deionized water.
e resulting solution was ltrated through lter paper.
Electrochemical measurements
In a complete potentiometric cell, the GEMI-ZnO-sem-
5 GEMI-ZnO-seml THF. e ZnO coated wires was
dipped twice into a prepared solution, aer each dip the
electrode was le to dry at room temperature, then the
electrode was conditioned into 1 × 10-3 M of GEMI stan-
dard solution for 24 hour prior to use. e membrane
was characterized by SEM (Zeiss Evo LS 10, Germany)
Figure 3.
Standard drug solutions
Stock standard solutions 0.01 M GEMI (Mw = 389.381
g/mol) was prepared by dissolving accurate weight in 5 mL
of 0.1 M NaOH and the volume was completed by deion-
ized water, this solution was kept in the dark at 4 °C. Work-
ing solutions ranging 0.5-10000 μM were prepared by serial
dilution of the stock solution by deionized water. e test-
ing series was prepared by adding adequate amount of (0.2
Figure 2: A,B) SEM at different magnications and view of the ZnO nanorodes grown on Ag wire hydrothermal aqueous chemical
method.
Figure 3: A,B) Presents ion selective membrane with KTFPB additive with different magnication.
• Page 53 •
Citation: Idress MO, Elbashir AA (2017) Development and Validation of Potentiometric ZnO Nanorods Modied
Ion Selective Electrode for Determination of Gemioxacin in Pharmaceutical Formulation. Current Trends Anal
Bioanal Chem 1(1):50-56
SCHOLARLY PAGES
Idress and Elbashir. Current Trends Anal Bioanal Chem 2017, 1(1):50-56
electrode potential was observed in pH range from 2 to
3 and decreased from pH 4 to 11, Figure 4. ese result
suggested that the inclusion complex of GEMI and HPβ-
CD was suitable in acidic media because GEMI contain-
ing primary amine group that capable to bind with pro-
tons presents in acidic media resulting positively charged
GEMI ion, which therefore can attracted by anionic tet-
raphenyl borate group present in the additive (KTFPB)
and hence facilities the inclusion between GEMI and
HPβ-CD [16,17,21].
Eect of volume of buer: e eect of volume of
buer on the potential response of the GEMI-ZnO-ISE
was studied using 1 × 10-4 M solutions in the range of
(0-10) mL using Na2HPO4/H3PO4 [pH 3; 0.2 M]. It was
found that the potential increased when buer adding to
GEMI solution without buer and the potential remains
constant with adding extra volume of buer as shown in
Figure 5.
Eect of temperature: e eect of temperature on
the potential response of the GEMI-ZnO-ISE was stud-
ied using 1 × 10-4 M solutions at the range of tempera-
ture (10-80) °C using thermometer presented in Figure
6. It reveals that the potential increased with increasing
temperature of drug solution this could be attributed to
potentiometric measurements is equilibrium controlled
[22], thus increasing solution temperature is resulting
faster equilibrium between the electrode surface and
GEMI solution.
Response time: e response time of potential of the
GEMI-ZnO-ISE was studied using 1 × 10-4 M solutions
in a period from 0 to 15 second. e potential readings
corresponding to time were recorded and plotted using
the proposed electrode in Figure 7. e sensor display
very fast and response within 2 second.
Electrode composition
e electrode shows linear Nernestian response over
a wide range of concentration 0.5-10000 μM, stable, sen-
sitive and very fast response. is attributed to electrode
compositions. e ZnO nanorods increased the surface
lective electrode was used in conjunction with Ag/AgCl ref-
erence electrode (inner and outer lling by KCl 3 M). e
electrochemical potential between the GEMI-ZnO-selec-
tive electrode as cathode and Ag/AgCl reference electrode
(Ω metrohm.Autolab, inner and outer lling by KCl 3 M) as
anode was measured with pH/mv meter (PHS-3E).
GEMI.TFPB - PVC || Test solution || Ag/AgCl (3
M.KCl)
e measured potential was plotted against the loga-
rithm of drug concentration. e electrode was washed
with deionized water blotted with tissue paper between
measurements.
Results and Discussions
Optimization conditions
Eect of pH: e eect of pH on the potential re-
sponse of the GEMI-ZnO-ISE was investigated using 1 ×
10-4 M solutions in pH range of 2.0-11.0 using Na2HPO4/
H3PO4 (0.2 M) as a buer solution. e potential read-
ings corresponding to dierent pH values were recorded
and plotted using the proposed electrode. Increasing in
pH value
potential (mv)
260
250
240
230
220
210
200
190
180
170
1 6 11 16
Figure 4: Optimization of pH for Gemi-TFPB-HPβ-CD, Gemi 1
× 10-4 M, at room temperature, time 2 sec.
volume of buffer (mL)
potential (mv)
0 2 4 6 8 10 12
90
85
80
75
70
65
60
55
50
45
40
Figure 5: Optimization of volume buffer for Gemi-TFPB-
HPβ-CD, Gemi 1 × 10-4 M, at room temperature, time, 2 sec,
pH 3.
temperature (°c)
potential (mv)
0 20 40 60 80 100
110
100
90
80
70
60
50
Figure 6: Optimization of temperature for Gemi-TFPB-HPβ-
CD, emi 1 × 10-4 M, time 2 sec and 5 mL pH 3.
• Page 54 •
Citation: Idress MO, Elbashir AA (2017) Development and Validation of Potentiometric ZnO Nanorods Modied
Ion Selective Electrode for Determination of Gemioxacin in Pharmaceutical Formulation. Current Trends Anal
Bioanal Chem 1(1):50-56
SCHOLARLY PAGES
Idress and Elbashir. Current Trends Anal Bioanal Chem 2017, 1(1):50-56
in CD cavity are displaced by more hydrophobic guest
molecules present in the solution to attain a non-polar/
non-polar association and decrease of CD ring strain re-
sulting in a more stable lower energy state [23]. On con-
structing an ISE, the amount of the sensing ionophore
in the electrode matrix should be sucient to obtain
reasonable complexation at the electrode surface that is
responsible for the electrode potential [24,25].
e function of KTFPB as lipophilic ionic additives
is to promote the interfacial ion exchange kinetics and
decrease the electrode resistance through enhancing the
ionic mobility in the electrode matrix. e response of
ISEs containing ionic sites can be distinguished wheth-
er the incorporated ionophore acts as an electrically
charged or uncharged carrier [26,27].
Statistical data
e analytical methods were validated with respect to
linearity, Limit of Detection (LOD), Limit of Quantica-
tion (LOQ) and precision according to ICH [28,29].
Calibration curve and statistical data for GEMI:
e measuring range of a potentiometric sensor was the
linear part of the calibration graph as shown in Figure 8.
e critical response coated wire sensor electrodes were
determined and the results were summarized in Table 1.
LOD and LOQ were determined using the formula: LOD
or LOQ = K.SD a/b, where K = 3.3 for LOD and 10 for
LOQ, SDa is the standard deviation of the intercept, and
b is the slope. the values of LOD and LOQ were found
to be 0.15 and 0.4546 μM respectively. e sensor show
nearly Nernestian response over the concentration range
0.5-10000 μM of the GEMI standard solution. Calibra-
tion graph slope for sensor electrode were 33.65 mV de-
area for distribution of the membrane compared if it di-
rectly attached to silver wire, thus increased the sensitiv-
ity of the electrode and decreases the response time [18].
HPβ-CD is used as sensing ionophore, the most import-
ant property of CDs is their ability to form supramolec-
ular inclusion complexes with many appropriately sized
organic ions and molecules in aqueous, non-aqueous
and mixed media [11]. e driving forces for the com-
plexation are non-covalent, including Van der Waals
forces and directed hydrogen bonding. Water molecules
time (s)
potential (mv)
0 2 4 6 8 10 12 14 16
190
185
180
175
170
165
160
Figure 7: Optimization of response time for Gemi-TFPB-
HPβ-CD, Gemi 1 × 10-4 M, time 2 sec and 5 mL pH 3.
-log conc
potential (mv)
0 1 2 3 4 5 6 7
250
200
150
100
50
0
y = 33.39x + 17.78
R
2
= 0.999
Figure 8: Calibration curve of Gemi-TFPB-HPβCD, Gemi 1
× 10-4 M, at room temperature, time 2 sec, 5 mL pH 3.
Table 1: Parameter for GEMI potentiometric method.
Parameter Value
Intercept ± SD 16.76 ± 1.53
Slop 33.65
Correlation coefcient (R2) linear 0.99929
Linear range (μM) 0.005-10000
LOD (μM) 0.1500
LOQ (μM) 0.4546
Response time 2 second
Life time > 6 months
*PDL 0.001 Μm
*PDL = Practical Detection Limit.
Table 2: Precision of the potentiometric method for GEMI determination.
Concentration Taken (-log C) Found (-log C) Recovery % ± RSD*
1 × 10-3 M 3 2.988 99.6 ± 1.12
5 × 10-5 M 4.3 4.356 101.3 ± 1.26
1 × 10-6 M 6 6.023 100.38 ± 1.74
*values are mean of three determinations; RSD = (SD /mean*100).
Table 3: Robustness of potentiometric method for GEMI de-
termination.
Parameter Value Recovery % ± RSD*
Standard conditions 99.1 ± 0.44
pH 2.5 98.5 ± 0.39
3.5 99.1 ± 0.45
Temperature (°C) 30 98.3 ± 0.29
40 96.2 ± 0.63
Volume of buffer (ml) 2 99.3 ± 0.93
8 98.7 ± 0.66
Reaction time (sec) 2 96.3 ± 0.74
10 98.6 ± 0.48
(*values are mean of 3 determinations); RSD = (SD /mean*100).
• Page 55 •
Citation: Idress MO, Elbashir AA (2017) Development and Validation of Potentiometric ZnO Nanorods Modied
Ion Selective Electrode for Determination of Gemioxacin in Pharmaceutical Formulation. Current Trends Anal
Bioanal Chem 1(1):50-56
SCHOLARLY PAGES
Idress and Elbashir. Current Trends Anal Bioanal Chem 2017, 1(1):50-56
Conclusion
It can be concluded that GEMI-ZnO-ISE oers a viable
technique for the direct determination of GEMI in phar-
maceutical preparations. e sensor allows simple, rapid,
and reproducible determination over a wide linear range of
concentration with the same sensitivity without the need of
complex sample manipulations. e sensor exhibits a good
selectivity towards the drug in the presence of various phar-
maceutical recipients, long life time and time-labor saving.
e procedure avoid the usual pretreatment steps neces-
sary for GEMI assays and presents some general advantages
over common chromatographic and spectroscopic proce-
dure, it makes use of less sophisticated equipments (there
for being easier to operate and providing lower cost of anal-
ysis) and surpasses color and turbidity problems associated
with suspensions and colloids.
Sensor accomplished LOD and LOQ of 0.15 μM,
0.4546 μM, respectively with a fast response time of less
than 5 seconds.
Acknowledgment
e authors gratefully acknowledge Prof. Omer Nur
from (Linköping University, Norrköping, Sweden) for
providing facilities to accomplish this work and Dr.
Manal Siyam for analysis samples by SEM in Naturkundi
Museum laboratories-Berlin-Germany.
References
1. Charan DC, Satyabrata S (2011) Simple and rapid spec-
terophotometric estimation of gemioxacin mesylate in bulk
andtablet formulations. International Journal of PharmTech
Research 3: 133-135.
2. Hannan P, Woodnutt G (2000) In vitro activity of gemioxa-
cin against human mycoplasmas. J Antimicrob Chemother
45: 367-369.
3. Thakre YM, Choudhary MD (2011) Synthesis, characteri-
zation and evaluation of derivative of Ciprooxacin (1-cy-
clopropyl-6-uoro-4-oxo-7-[4-(phenyl carbonyl) piperaz-
in-1-yl]-1, 4-dihydroquinoline-3-carboxylic acid) and their
complexes. J Chem Pharm Res 3: 390-398.
4. Szejtli J (1988) Cyclodextrin Technology. In: Kluwer Aca-
demic Publishers, Dordrecht, Netherlands, 1-78.
5. Sugumaran M, Jotheeswari D (2011) RP-HPLC meth-
od for the determination of gemioxacin mesylate in bulk
and pharmaceutical formulation. Int J Pharm Sci Rev Res
6: 18-20.
cade-1. e electrodes exhibited a fast dynamic response
of 2 s for a period for more than 6 months without signif-
icant change in the electrodes parameters.
Accuracy and precision of the potentiometric meth-
od: e accuracy and precision of the proposed method
was determined at three concentration levels of GEMI
by apply three replicate samples of each concentration.
e standard deviations for the results did not exceed 2%
are listed in Table 2, indicating high reproducibility of
the results and precision of the method. is good level
of precision was suitable for quality control analysis of
GEMI and in the pharmaceutical formulations.
Robustness of potentiometric method for GEMI:
Robustness was examined by evaluating the inuence of
small variation in the method variables on its analytical
performance. In these experiments, one parameter was
changed, whereas the others were kept unchanged, and
the recovery percentage was calculated each time. It was
found that small variables did not signicantly aect the
procedures, recovery values were shown in Table 3.
Analysis of pharmaceutical formulations: Proposed
methods were applied to the pharmaceutical formu-
lations and indicate the high accuracy of the proposed
method for determination of GEMI. e proposed
method has advantage of being virtually free from inter-
ferences by excipients. e percentage was 106.43 ± 0.51.
Recovery study of the potentiometric method: To
a xed amount of the drug in the dosage form and pure
drug (the standard) were added at ve dierent levels
and the total was found by the proposed method each
test was performed in triplicate. Table 4 revealing good
accuracy and no interference from excipients. Recovery
was calculated as the amount found/amount taken × 100.
values are mean ± R.S.D. for three determinations.
e sensitivity: e sensitivity was tested by adding
some inorganic salts and diluted acids and bases, it was
found that the electrode shows excellent sensitivity to-
ward testing species with RSD less than 2%.
Reproducibility: e electrode response shows ex-
cellent repeatability during analysis and very stable re-
sponse with intraday RSD did not exceeded 2%, and in-
ters day analysis with RSD less than 5%.
Table 4: Recovery of the potentiometric method of GEMI.
Sample content M Standard added M p [Concentration] Found log [Concentration] Recovery (% ± RSD)*
1 × 10-4 1 × 10-4 3.70 4.14 111.8 ± 0.64
1 × 10-4 2 × 10-4 3.52 3.64 103.41 ± 1.81
1 × 10-4 3 × 10-4 3.40 3.34 98.23 ± 0.77
1 × 10-4 4 × 10-4 3.30 3.16 95.76 ± 0.94
1 × 10-4 5 × 10-4 3.22 3.07 95.28 ± 0.83
• Page 56 •
Citation: Idress MO, Elbashir AA (2017) Development and Validation of Potentiometric ZnO Nanorods Modied
Ion Selective Electrode for Determination of Gemioxacin in Pharmaceutical Formulation. Current Trends Anal
Bioanal Chem 1(1):50-56
SCHOLARLY PAGES
Idress and Elbashir. Current Trends Anal Bioanal Chem 2017, 1(1):50-56
6. Doyle E, Fowles SE, McDonnell DF, et al. (2000) Rapid de-
termination of gemioxacin in human plasma by high-per-
formance liquid chromatography-tandem mass spectrome-
try. J Chromatogr B Biomed Sci Appl 746: 191-198.
7. Elbashir AA, Saad B, Salhin A, et al. (2008) Validated Sta-
bility Indicating Assay of Gemioxacin and Lomeoxacin
in Tablet Formulations by Capillary Electrophoresis. J Liq
Chromatogr Relat Technol 31: 1465-1477.
8. Robledo VR, Smyth WF (2008) A study of the analytical
behaviour of selected new molecular entities using electro-
spray ionisation ion trap mass spectrometry, liquid chroma-
tography, gas chromatography and polarography and their
determination in serum at therapeutic concentrations. Anal
Chim Acta 623: 221-230.
9. Ebraheem SAM, Elbashir AA, Aboul-Enein HY (2011)
Spectrophotometric methods for the determination of gemi-
oxacin in pharmaceutical formulations. Acta Pharm Sinica
B 1: 248-253.
10. Tekkeli SEK, Onal A (2011) Spectrouorimetric Methods
for the Determination of Gemioxacin in Tablets and Spiked
Plasma Samples. J Fluoresc 21: 1001-1007.
11. Dsugi NFA, Elbashir AA, Suliman FEO (2015) Supra mo-
lecular interaction of gemioxacin and hydroxyl propyl β-cy-
clodextrin spectroscopic characterization, molecular mod-
eling and analytical application. Spectrochim Acta A Mol
Biomol Spectrosc 151: 360-367.
12. Zha F, Zhao W, Xiong W (2012) Chemiluminescence de-
termination of gemioxacin based on diperiodatoargentate
(III)-sulphuric acid reaction in a micellar medium. Lumines-
cence 28: 108-113.
13. Mahajan RK, Kaur I, Sharma V, et al. (2002) Sensor for
Silver(I) Ion Based on Schiff-base-p-tertbutylcalix[4]arene.
Sensors 2: 417-423.
14. Mascini M, Pallozzi F (1974) Selectivity of neutral carrier-
pvc membrane electrodes. Anal Chim Acta 73: 375-382.
15. Ganjali MR, Norouzi P, Rezapour M (2006) Encyclopedia of
Sensors, Potentiometric Ion Sensors. American Scientic
Publisher 8: 197-288.
16. Al-Mohaimeed M, Al-Tamimi SA, Alarfaj NA, et al. (2012)
New Coated Wire Sensors for Potentiometric Determina-
tion of Gemioxacin in Pure Form, Pharmaceutical For-
mulations and Biological Fluids. Int J Electrochem Sci 7:
12518-12530.
17. Abo-talib NF (2013) Ion Selective Electrodes for Stabili-
ty-Indicating Determination of Gemioxacin Mesylate. Anal
Bioanal Electrochem 5: 74-86.
18. Qin Y, Wang XD, Wang ZL (2008) Microbre-nanowire hy-
brid structure for energy scavenging. Nature 451: 809-813.
19. Vayssieres L (2003) Growth of Arrayed Nanorods and
Nanowires of ZnO from Aqueous Solutions. Advanced Ma-
terials 5: 464-466.
20. Anees A, Ansari M, Alhoshan MS, et al. (2010) Nanostruc-
tured Metal Oxides Based Enzymatic Electrochemical Bio-
sensors. In Tech Rijeka 1: 23-46.
21. Maha ET, Sawsan R, Magda EM, et al. (2010) Construction
and Optimization of Selective Membrane Electrodes for Deter-
mination of Doxepin Hydrochloride in Pharmaceutical Prepa-
rations and Biological Fluids. J Kor Chem Soc 54: 198-207.
22. Zhang J, Harris AR, Cattrall RW, et al. (2010) Voltammetric
Ion-Selective Electrodes for the Selective Determination of
Cations and Anions. Anal Chem 82: 1624-1633.
23. Suliman FEO, Elbashir AA, Schmitz OJ (2015) Study on
the separation of ooxacin enantiomers by hydroxyl-pro-
pyl-β-cyclodextrin as a chiral selector in capillary electro-
phoresis: a computational approach. Journal of Inclusion
Phenomena and Macrocyclic Chemistry 83: 119-129.
24. Elbashir AA, Dsugi NFA, Aboul-Enein HY (2014) Supra-
molecular Study on the Interaction Between Ooxacin and
Methyl β-Cyclodextrin by Fluorescence Spectroscopy and
its Analytical Application. J Fluoresc 24: 355-361.
25. Khaled E, Hassan HNA, Mohamed GG, et al. (2010) β-Cyclo-
dextrin-based potentiometric sensors for ow-injection deter-
mination of acetylcholines. Int J Electrochem Sci 5: 448-458.
26. Bakker E, Pretsch E (1995) Lipophilicity of tetraphenylbo-
rate derivatives as anionic sites in neutral carrier-based
solvent polymeric membranes and lifetime of correspond-
ing ion-selective electrochemical and optical sensors. Anal
Chim Acta 309: 7-17.
27. Hansen AJ (1981) Extracellular ion concentrations during
cerebral ischemia. In: Zeuthen T, The Application of Ion-Se-
lective Microelectrodes. Elsevier, New York, 239-254.
28. Topic Q2 (R1) (2005) Validation of analytical procedures:
Text and morphology. International Conference of Harmo-
nization (ICH).
29. (1995) ICH-Q2A guideline for industry March. Text on vali-
dation of analytical procedures.
