Development and
Validation of Spectrophotometric Determination of Cefpodoxime Proxetil in Pure
Form and Pharmaceutical Formulation through Ion-Pair Complex Formation Using
Bromocresol Purple
Abdul
Aziz Ramadan1*, Hasna Mandil, Rasha Shamseh
Department of Chemistry,
Faculty of Science, University of Aleppo, Syria
*Corresponding Author E-mail: dramadan@scs-net.org
ABSTRACT:
A simple, direct and accurate
spectrophotometric method has been developed for the determination of
cefpodoxime proxetil (CEFP) in pure form and pharmaceutical formulations by
complex formation with bromocresol purple (BCP). The method involves the
formation of yellow ion-pair complexes between BCP reagent and CEFP in
chloroform. The two formed complexes ([CEFP]: [BCP] and [CEFP]: [BCP]2)
have maximum absorption at λmax 414 nm. The proposed method was
validated for specificity, linearity, precision and accuracy, repeatability,
sensitivity (LOD and LOQ), robustness and solution stability with an average
recovery of 99.2-101.0%.The formed complexes ([CEFP]:[BCP] and [CEFP]:[BCP]2)
were measured against the reagent blank prepared in the same manner. Variables
were studied in order to optimize the reaction conditions. Molar absorptivity
(ε) for two complexes were 10500 and 15700 L.mol-1.cm-1,
respectively. Beer’s law was obeyed in the concentration range of 0.5576-5.576
and 5.576-55.760 μg/ml in the present of 2x10-4 and 1x10-3
mol/l of BCP, respectively, with good correlation coefficient (R2=
0.9988 and R2= 0.9995, respectively). The relative standard
deviation did not exceed 4.4%. The limit of detection (LOD) and the limit of
quantification (LOQ) were 0.083 and 0.25 μg/ml, respectively. The
developed method is applicable for the determination of CEFP in pure and
different dosage forms with the average assay of marketed formulations 91.6 to
106.2%, and the results are in good agreement with those obtained by the
RP-HPLC reference method.
KEYWORDS: Direct
spectrophotometric method, Cefpodoxime proxetil, Bromocresol purple,
Ion-pair complex.
INTRODUCTION:
Scheme 1: Chemical structure of
cefpodoxime proxetil (CEFP).
Cefpodoxime Proxetil (CEFP) is
a third generation cephalosporin antibiotic indicated for the treatment of
patients infected with susceptible strains of microorganisms which include a
wide range of gram-positive and gram-negative bacteria. It is commonly used to
treat acute otitis media, pharyngitis, and sinusitis. The molecular formula of
CEFP is C21H27N5O9S2 and
the molecular weight is 557.6 g/mol. It is freely soluble in dehydrated
alcohol, acetonitrile, methanol and very slightly soluble in water 1-3,
see Scheme 1.
Scheme 2: Chemical structure of
Bromocresol purple (C21H16Br2O5S).
Bromocresol purple C21H16Br2O5S
(BCP), acts as a weak acid in solution. It can thus be in protonated or
deprotonated form, appearing yellow or purple, respectively, mol. mass 540.22 g4,
see scheme 2. Bromocresol purple has been used as a reagent to form ion pair
complexes with drugs as gatifloxacin5.
A simple, sensitive, accurate
and rapid UV-Vis spectrophotometric methods have been developed for the
estimation of cefpodoxime proxetil in bulk drug and in pharmaceutical dosage
form, which shows maximum absorbance at 415 and 425 nm for ion-pair complexes between
cefpodoxime proxetil with BCP and bromocresol green, receptively, by extraction
it in chloroform6.
Various spectrophotometric
methods 6-24 have been reported for the determination of cefpodoxime
proxetil in pure as well as in dosage forms. Most spectrophotometric methods
employ extraction procedures. The complex extraction technique has some
difficulties and inaccuracies due to incomplete extraction or the formation of
emulsions between the hydrocarbon solvent and the basic compound-containing solution.
In response to the problems resulting from the extraction of the complex, it is
better to determine formed complex without extraction 25. Also, none
of the direct methods reported in the literature are based on the formation of
a complex between BCP and CEFP.
Several analytical methods for
the determination of cefpodoxime proxetil have been reported including
high-performance liquid chromatography (HPLC)26-30 and
electrochemical methods31-33.
In this study, a
extraction-free spectrophotometric method for determination of CEFP through
ion-pair complex formation with BCP was developed.
MATERIALS AND
METHODS:
Instruments
and apparatus:
Spectrophotometric
measurements were made in Spectro scan 80 DV UV-VIS spectrophotometry with 1 cm
quartz cells. An ultrasonic processor model Powersonic 405 was used to sonicate
the sample solutions. The diluter pipette model DIP-1 (Shimadzu), having 100
μl sample syringe and five continuously adjustable pipettes covering a
volume range from 10 to 5000 μl (model Piptman P, GILSON). Centrifuge
(Centurion Scientific Ltd., Model: K2080-Manufactured in the United Kingdom)
was used for the preparation of the experimental solutions. SARTORIUS TE64
electronic balance was used for weighing the samples.
Reagents:
Cefpodoxime proxetil (96.138%)
was supplied by Virchow group company (INDIA), its purity as cefpodoxime was
(73.7%), (Mfg. 07/2015, Exp. 07/2018). Bromocresol purple (99%) of analytical
grade and chloroform of extra pure were from MERCK. All solvents and reagents
were analytical grade chemicals.
Stock
standard solution of bromocresol purple (BCP) 1x10-2 mol/l:
Accurately weighed 136.42 mg
of BCP was dissolved in chloroform into a volumetric flask (25 ml) and diluted
up to mark with chloroform.
Stock
standard solution of CEFP 1x10-3 mol/l:
This solution was prepared by
dissolving 14.50 mg of CEFP in chloroform into a volumetric flask (25 ml) and
diluted up to mark with chloroform.
Working
standard solutions of CEFP:
The stock solution was further
diluted daily just before the use to obtain working solutions of CEFP in the
concentrations: 1.0, 2.0, 4.0, 6.0, 8.0, 10, 20, 40, 60, 80 and 100 μM (0.5576, 1.1152, 2.2304, 3.3456, 4.4608, 5.576, 11.152, 22.304,
33.456, 44.608 and 55.760 μg/ml of CEFP or 0.4275, 0.8549,
1.7098, 2.5647, 3.4197, 4.2746, 8.5492, 17.0983, 25.6475, 34.1966, and
42.7458 of CEF) by transferring different aliquots from stock standard
solution: 10, 20, 40, 60, 80, 100, 200, 400, 600, 800 and 1000 μl into 10
ml volumetric flasks, then 0.20 and 1.00 ml from stock standard solution of BCP
(1x10-2 mol/l) for concentrations 1.0–10.0 and 10.0-100.0 μM,
respectively, were added, and diluted to 10 ml with chloroform.
Sample
preparation:
Commercial formulations (as a
tablet) were used for the analysis of CEFP. The pharmaceutical formulations
subjected to the analytical procedure were:
(1) Oracef tablets,
El-Saad pharma, Aleppo–SYRIA, each tablet contains 100 and 200 mg of
cefpodoxime (CEF) (Mfg. 12/2013, Exp. 12/2017 and Mfg. 09/2014, Exp. 09/2018,
respectively).
(2) Oraxime tablets,
Asia pharmaceutical industries, Aleppo–SYRIA, each tablet contains 100 and 200
mg of CEF (Mfg. 12/2013, Exp. 12/2016 and Mfg. 11/2014, Exp. 11/2017,
respectively).
(3) Oraluxe tablets,
ALPHA. Aleppo pharmaceutical industries, Aleppo-SYRIA, each tablet contains 100
and 200 mg of CEF (Mfg. 01/2015, Exp. 01/2018 for two pharmaceuticals).
Stock
solutions of pharmaceutical formulations:
20 tablets of each studied
pharmaceutical formulation were weighed accurately, crushed to a fine powder
and mixed well. An amount of the powder equivalent to the weight of one tablet
was solved in chloroform using ultrasonic for 10 min, 20 ml of chloroform was
added, filtered over a 25 ml flask and washed by the same solvent, then diluted
to 25 ml with chloroform. This solution contains the follows: 4 and 8 mg/ml of
CEF for all studied pharmaceutical formulations contain 100 and 200 mg/tab,
respectively.
Working
solutions of pharmaceuticals:
Five solutions were prepared
daily by diluting 50 and 25 μl from a stock solution of pharmaceutical
formulations for contents: 100 and 200 mg/tab, respectively. Then adding
1 ml from a stock standard solution of BCP and adjusting the volume up to 10 ml
with chloroform (these solutions contain 20 μg/ml of CEF
(26.09 μg/ml of CEFP); test solutions).
Procedure:
A solution (10 ml) containing
an appropriate concentration of CEFP (or working solutions of pharmaceuticals)
with appropriate amount of BCP in chloroform was ready for spectrophotometric
measurement at λmax 414 nm.
RESULTS AND
DISCUSSION:
The different experimental
parameters affecting the spectrophotometric determination of CEFP through
ion-pair complex ([CEFP]:[BCP]2) formation with BCP in chloroform
were studied for determining the optimal conditions.
Spectrophotometric
results:
UV-Vis spectra of CEFP, BCP
and the formed complexes CEFP: BCP solutions (using pure chloroform or 2x10-4M
and 1x10-3M of BCP in chloroform as blank) were obtained. CEFP
solutions do not absorb in the range 360-600 nm. BCP solutions have small
absorption at λmax 410 nm, molar absorptivity (ε)=470 L.
mol-1. cm-1. [CEFP]: [BCP] and [CEFP]:[BCP]2
complexes solutions have maximum absorption at λmax 414 nm,
(ε for two complexes were 10500 and 15700 L. mol-1. cm-1,
respectively), see fig. 1.
The effect of
time and temperature:
The effect of time and
temperature on the complex ([CEFP]:[BCP]2) formation was studied
within the ranges 5-120 min and 15-25oC. It was found that the
formed complex wasn't affected by time or temperature at those ranges.
The effect of
BCP concentration:
The effect of BCP
concentration on complex ([CEFP]:[BCP]2) formation was investigated.
It was observed that the absorbance of the formed complex increased coinciding
with increasing the ratio of CBCP: CCEFP until the ratio
(2:1), then slowly increased until the absorbance became a quasi-static at
ratio more than 10.
Composition of
CEFP: BCP complexes:
Fig. 1: UV-Vis spectra in
chloroform of : 1-1.0x10-4 mol/l of CEFP; 2-1.0x10-4
mol/l of BCP; 3-1.0x10-4 mol/l ion-pair complex [CEFP]:[BCP] (1.0x10-4
mol/l of BCP with 4.0x10-4 mol/l of CEFP); 4 and 5-1.0x10-4
mol/l ion-pair complex [CEFP]:[BCP]2 (1.0x10-4 mol/l of
CEFP with 1.0x10-3 mol/l of BCP); 1-4: Blank is chloroform; 5-Blank
is 1.0x10-3 mol/l of BCP, ℓ =1 cm.
The composition of CEFP:BCP
complexes were determined by the molar ratio method and Job's method of
continuous variation.
Molar ratio method:
The stoichiometry of CEFP: BCP
complexes were studied by molar ratio method according to following equation: Amax=
f([BCP]/[CEFP]) at λmax 414 nm. It confirmed that the binding
ratio of CEFP: BCP complexes are equal to (1:1 and 1:2); where the
concentration of CEFP was constant (100 μM) and the concentrations of BCP
changed from 0 to 400 μM (fig. 2). The formation constant of the ion pair
complexes [CEFP]:[BCP] and [CEFP]:[BCP]2 are 2.23x105 and
2.71x106, respectively.
Fig. 2: Molar ratio method to
calculate binding ratio of CEFP: BCP complexes at λmax=414 nm ([CEFP]= 100
μM, blank is chloroform, ℓ =1 cm).
Job’s method of
continuous variation:
Continuous
variation was utilized to check the composition of CEFP: BCP complexes at
λmax 414 nm. The absorbance of the complexes were plotted
against the mole fraction [BCP]/([CEFP]+[BCP]), where [CEFP]+[BCP]=200 μM.
The plot reached maximum values at a mole fraction of 0.5 and 0.67, see fig. 3.
This indicated complexes formation (CEFP: BCP) in the ratio of (1:1 and 1:2).
The formation constant of the ion-pair complexes [CEFP]:[BCP] and [CEFP]:[BCP]2
are 2.25x105 and 2.76x106, respectively.
The optimum conditions for
spectrophotometric determination of CEFP through ion-pair complex formation
using BCP in chloroform are shown in table 1.
Fig. 3: Job's method of
continuous variation to calculate binding ratio of CEFP: BCP complexes at
λmax 414 nm ([CEFP]+[BCP]=200 μM, blank is chloroform, ℓ =1
cm).
Table 1: The optimum conditions
for spectrophotometric determination of CEFP by complexes formation with BCP in
chloroform.
Parameters |
Operating modes |
Temperature of solution |
20±5oC |
CBCP: CCEFP, M |
≥10 |
Solvent |
chloroform |
Stability |
2 h |
λmax of CEFP: BCP complexes |
414 nm |
Light path (ℓ) |
1.0 cm |
Spectra range |
300–600 nm |
Mechanism of
reaction:
Anionic dyes such as BCP form
ion-pair complexes with the positively charged nitrogen-containing molecule.
The colour of such dyes is due to the opening of lactoid ring and subsequent
formation of the quinoid group (deprotonated). CEFP is protonated and forms
yellow ion-pair complexes [CEFP]:[BCP] and [CEFP]:[BCP]2 with the
dye. Each drug-dye complex with two oppositely charged ions (positive on the
drug and negative on the dye) behaves as a single unit held together by an
electrostatic binding. The suggested mechanism of CEFP: BCP ion-pair complexes
formation are shown in Scheme 3.
Calibration
curve:
The calibration curve of CEFP
in pure form through complexation with BCP showed excellent linearity over the
concentration range of 1.0-10.0
μM and 1.0-100.0 μM (or 0.5576–5.576 μg/ml and 0.5576-55.760 μg/ml), see fig. 4 and 5. Regression equations
at λmax 414 nm were as the follows:
y=0.0156x+0.0015; R2=0.9995
(or y=0.0279x+0.0009; R2=0.9995) (I)
y=0.0158x+0.0039; R2=0.9988
(or y=0.0282x+0.0023; R2=0.9988) (II)
The spectra characteristics of
the method such as the molar absorptivity (ε), Beer's law, regression
equation at λmax 414 nm (y=a.x+b); where y=absorbance, a=slope,
x=concentration of CEFP in μM or μg/ml,b=intercept, the correlation
coefficient, limit of detection (LOD) and limit of quantification (LOQ) are
summarized in table 2.
Analytical results:
Spectrophotometric
determination of CEFP through complexation with BCP in chloroform within
optimal conditions using calibration curve was applied. The results, summarized
in table 3, showed that the determined concentration of CEFP was rectilinear
over the range of 1.0 to 100.0 μM or 0.5576 to 55.760 μg/ml with
relative standard deviation (RSD) not more than 4.4%. The results obtained from
the developed method have been compared with the official RP-HPLC method 26
and good agreement was observed between them (table 3).
Scheme 3: Mechanism of
[CEFP]:[BCP] and [CEFP]:[BCP]2 complexes formation.
Fig. 4: Spectra of [CEFP]:[BCP]2
complex in present 1.0×10-3 M of BCP; where CCEFP as the
follows: 0.5576, 1.1152, 2.2304, 3.3456, 4.4608, 5.576,
11.152, 22.304, 33.456, 44.608 and 55.760 μg/ml for curves (1-11)
{Blank is BCP solution in chloroform 2x10-4 and 1x10-3M
for curves (1-6 and 1-11, respectively); ℓ = 1 cm}.
Fig. 5: Calibration curve for
determination of CEFP according to optimal conditions at λmax 414 nm (in
present of 1×10-3 M of BCP) where CCEFP: 0.5576 - 55.760
μg/ml (a) and (in present of 2×10-4 M of BCP) where CCEFP:
0.5576 – 5.576 μg/ml (b) {Blank is BCP solution in chloroform 1x10-3
M (a) and 2x10-4M (b); ℓ = 1 cm}.
Table 2: The parameters
established for spectrophotometric determination of CEFP by complex formation
with BCP in chloroform
Parameters |
Operating values |
Molar absorptivity of [CEFP]:[BCP] complex (ε1 ), L. mol-1. cm-1 |
10500 |
Molar absorptivity of [CEFP]:[BCP]2 complex (ε2 ), L. mol-1. cm-1 |
15700 |
Regression equation for [CEFP]:[BCP]2 at λmax =414 nm (CCEFP= 1.0-10.0 μM): |
|
Slope |
0.0158 |
Intercept |
0.0039 |
Correlation coefficient (R2) |
0.9988 |
Regression equation for [CEFP]:[BCP]2 at λmax =414 nm (CCEFP= 1.0-100.0 μM): |
|
Slope |
0.0156 |
Intercept |
0.0015 |
Correlation coefficient (R2) |
0.9995 |
Regression equation for [CEFP]:[BCP]2 at λmax =414 nm (CCEFP= 0.5576-55.760 μg/ml): |
|
Slope |
0.0279 |
Intercept |
0.0009 |
Correlation coefficient (R2) |
0.9995 |
Beer’s Law Limit, for CCEFP by μM |
1-100 |
Beer’s Law Limit, for CCEFP by μg/ml |
0.5576-55.760 |
RSD% |
4.4 |
LOD(3.3SD), for CCEFP by μg/ml |
0.083 |
LOQ (10SD), for CCEFP by μg/ml |
0.25 |
n=5, t=2.776.
Table 3: Spectrophotometric
determination of CEFP through complex formation with BCP within optimal
conditions using calibration curve in chloroform
Xi, μg/ml (Taken) |
* μg/ml (mean±SD) |
mg/ml |
|
RSD % |
* RP-HPLC 26 |
0.5576 |
0.577± 0.025 |
0.011 |
0.577± 0.031 |
4.4 |
0.559 |
1.1152 |
1.258± 0.050 |
0.023 |
1.258± 0.062 |
4.0 |
1.120 |
2.2304 |
2.369± 0.088 |
0.039 |
2.369± 0.109 |
3.7 |
2.210 |
3.3456 |
3.516± 0.120 |
0.053 |
3.516± 0.148 |
3.4 |
3.314 |
4.4608 |
4.412± 0.132 |
0.059 |
4.412± 0.164 |
3.0 |
4.600 |
5.576 |
5.774± 0.173 |
0.077 |
5.774± 0.215 |
3.0 |
5.592 |
11.152 |
11.258± 0.326 |
0.146 |
11.258± 0.405 |
2.9 |
11.182 |
22.304 |
21.473± 0.601 |
0.269 |
21.473± 0.746 |
2.8 |
22.310 |
33.456 |
33.301± 0.866 |
0.387 |
33.301± 1.075 |
2.6 |
33.415 |
44.608 |
45.129± 1.128 |
0.505 |
45.129± 1.400 |
2.5 |
44.620 |
55.760 |
55.882± 1.341 |
0.600 |
55.882± 1.665 |
2.4 |
55.695 |
* n=5, t= 2.776
METHOD
VALIDATION:
The developed method for
estimation of CEFP has been validated in accordance with the International
Conference on Harmonization guidelines (ICH) 34. The proposed method
has been validated for determination of CEF in tablet dosage form. Calibration
curves were constructed and the regression equations were calculated. The
calibration curves were plotted over the concentration range 0.5576-55.760
μg/ml for CEFP. Accurately measured working standard solutions of CEFP
(0.5576, 1.1152, 2.2304, 3.3456, 4.4608, 5.576, 11.152, 22.304, 33.456, 44.608
and 55.760 μg/ml) were analysed under the operating conditions.
Specificity:
Specificity test determines
the effect of excipients on the assay result. To determine the specificity of
the method, standard solution of CEFP, commercial product solution and blank
solutions were analyzed. The results of the tests proved that the components
other than the drug did not produce any interfere. The standard spectra
no interference from excipients present in the formulation indicate specific of
the method.
Linearity:
Several aliquots of a standard
stock solution of CEFP were taken in different 10 ml volumetric flask and
diluted up to the mark with chloroform such that their final concentrations
were 0.5576-55.760 μg/ml for CEFP. Absorbance was plotted against the
corresponding concentrations to obtain the calibration graph, see fig. 5.
Linearity equations obtained were y = 0.0279x+0.0009 for the range
0.5576-55.760 μg/ml (R2=0.9995) .
Precision and
accuracy:
The precision and accuracy of
proposed method were checked by recovery study by addition of standard drug
solution to pre-analyzed sample solution at three different concentration
levels (80%, 100% and 120%) within the range of linearity for CEFP. The basic
concentration level of sample solution selected for spiking of the CEFP
standard solution was 11.152 μg/ml. The proposed method was validated
statistically and through recovery studies and was successfully applied for the
determination of CEFP in pure and dosage forms with average percent recoveries
ranged from 99.2% to 101.0%, see table 4.
Table 4: Results of recovery
studies
Level |
% Recovery |
80% (n=5) |
99.2 |
100% (n=5) |
100.8 |
120% (n=5) |
101.0 |
The results of recovery
studies indicate that the proposed method is highly accurate. The results
obtained for CEFP were comparable with the corresponding labeled amounts. No
interference of the excipients with the absorbance of interest appeared; hence,
the proposed method is applicable for the routine simultaneous estimation of
CEFP in pharmaceutical dosage forms.
Repeatability:
The repeatability was
evaluated by performing 10 repeat measurements for 11.152 μg/ml of CEFP
using the studied spectrophotometric method under the optimum conditions. The
found amount of CEFP (±SD) was 11.181±0.33 μg/ml and the percentage
recovery was found to be 100.9±2.9 with RSD of 0.029. These values indicate
that the proposed method has high repeatability for CEFP analysis.
Sensitivity
(limit of detection [LOD] and limit of quantitation [LOQ]):
The sensitivity of the method
was evaluated by determining the LOD and LOQ. The values of LOD and LOQ for
CEFP are 0.083 and 0.25 μg/ml, respectively.
Robustness:
The robustness of the method
adopted is demonstrated by the constancy of the absorbance with the deliberated
minor change in the experimental parameters such as the change in the
concentration of excipients, BCP (±5%), temperature (±5oC) and
reaction time (30 min).
Solution stability:
The difference in the initial
value of percentage assay and the values obtained at 5, 15, 30, 60, 90
and 120 min (in 15-25oC) of percentage assay should not
be more than 2.4%. The assay obtained at different time intervals were compared
with the initial assay values. Solution stability period for sample solution
and standard solution was determined. Standard and sample solutions were stable
till 120 min. Solution stability period for standard preparation and sample
preparation were found to be within the acceptance criteria.
Applications:
The developed
spectrophotometric method was applied to determine CEFP in some pharmaceutical
preparations through complex formation by BCP in chloroform according to the
optimal conditions. The amount (m) of CEFP in one tablet was calculated from
the following relationship: m = h. m', where: m' is the amount of CEFP in
tablet calculated according to the regression equation (II), h conversion
factor is equal to 2.5 and 5.0 for pharmaceutical formulations contain 100 and
200 mg/tab, respectively. The results of quantitative analysis for CEFP in
pharmaceutical preparations were summarized in Tables 5.
Table 5: Determination of CEFP,
as cefpodoxime (CEF), in some Syrian pharmaceutical preparations using
spectrophotometric method through complex formation with BCP in chloroform,
λmax 414 nm
* (Assay%), by RP-HPLC 26 |
Assay% |
RSD% |
*mean±SD
(as CEF), mg/tab. |
Label claim of CEFP as CEF, mg/tab. |
Tablet dosage form |
105.8 |
106.2 |
2.4 |
106.2±2.55 |
100 |
Oracef |
91.9 |
91.6 |
2.5 |
183.2±4.58 |
200 |
|
102.1 |
102.4 |
2.4 |
102.4±2.46 |
100 |
Oraxime |
101.9 |
101.9 |
2.2 |
203.8±4.48 |
200 |
|
93.7 |
93.5 |
2.3 |
93.5±2.15 |
100 |
Oraluxe |
102.4 |
102.5 |
2.2 |
205.0±4.51 |
200 |
* n=5,
Assay=(found mean/label claim)x100.
The proposed method was
simple, direct, specific and successfully applied to the determination of CEFP
in pharmaceuticals without any interference from excipients. Average assay of
marketed formulations ranged between 91.6 to 106.2%. The results obtained by
this method agree well with the contents stated on the labels and were
validated by RP-HPLC method 26.
CONCLUSION:
The developed
spectrophotometric method is simple, direct (extraction-free) and
cost-effective for the determination of CEFP in pure and tablet dosage forms.
This method is based on formation of two ion-pair complexes between CEFP and
BCP in chloroform ([CEFP]:[BCP] and [CEFP]:[BCP]2). Beer’s law in
the optimum experimental conditions using [CEFP]:[BCP]2 complexes is
valid within a concentration range of 0.5576-55.760 μg/ml. The developed
method is applied for the determination of CEFP in pure and its commercial
tablets without any interference from excipients with the average assay of
marketed formulations between 91.6 to 106.2%.This method was validated for
specificity, linearity, precision and accuracy, repeatability, sensitivity (LOD
and LOQ), robustness and solution stability with an average recovery of
99.2-101.0%. No interference of the excipients; hence, the proposed method is
applicable for the routine estimation of CEFP in pharmaceutical dosage forms.
CONFLICT OF
INTERESTS:
The authors have
declared that no conflict of interests exists.
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ICH: Proceedings of the International Conference on Harmonization of
Technical Requirement of Registration of Pharmaceuticals for Human Use (ICH
Harmonized Tripartite Guidelines); 2000.
Received on
03.01.2017
Modified on 30.01.2017
Accepted on
22.02.2017 © RJPT All
right reserved
Research J. Pharm. and Tech.
2017; 10(3): 843-851.
DOI: 10.5958/0974-360X.2017.00158.5