DEVELOPMENT AND VALIDATION OF SPECTROPHOTOMETRIC DETERMINATION OF
CEFPODOXIME PROXETIL IN PURE AND TABLET DOSAGE FORMS THROUGH ION-PAIR
COMPLEX FORMATION USING BROMOTHYMOL BLUE
Original Article
ABDUL AZIZ RAMADAN
1*
, HASNA MANDIL, RASHA SHAMSEH
Department of Chemistry, Faculty of Science, University of Aleppo, Syria
Email: dramadan@scs-net.org
Received: 26 Apr 2016 Revised and Accepted: 20 June 2016
ABSTRACT
Objective: A simple, direct and accurate spectrophotometric method has been developed for the determination of cefpodoxime proxetil (CEFP) in
pure and pharmaceutical formulations by complex formation with bromothymol blue (BTB).
Methods: The method involves the formation of yellow ion-pair complexes between BTB reagent and CEFP in chloroform. The two formed
complexes ([CEFP]: [BTB] and [CEFP]: [BTB]2) have maximum absorption at λmax 422 nm. The proposed method was validated for specificity,
linearity, precision and accuracy, repeatability, sensitivity (LOD and LOQ) and robustness with an average recovery of 99.0-101.4%.
Results: The formed complex ([CEFP]: [BTB]2) was 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 8100 and 12600 L. mol
-1
. cm
-1
, respectively. Beer’s law was obeyed in
the concentration range of 0.5576-55.760 μg/ml in the present of 1x10
-3
mol/l of BTB with good correlation coefficient (R
2
= 0.9995). The relative
standard deviation did not exceed 4.7%. The limit of detection (LOD) and the limit of quantification (LOQ) were 0.088 and 0.27 μg/ml, respectively.
Conclusion: The developed method is applicable for the determination of CEFP in pure and different dosage forms with the average assay of
marketed formulations 99.5 to 103.2%, and the results are in good agreement with those obtained by the RP-HPLC reference method.
Keywords: Direct spectrophotometric method; Cefpodoxime proxetil; Bromothymol blue; Ion-pair complex.
© 2016 The Authors. Published by Innovare Academic Sciences Pvt Ltd. This is an open access article under the CC BY license (http://creativecommons.org/licenses/by/4.0/)
INTRODUCTION
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. It is chemically
described as (RS)-1(isopropoxycarbonyloxy) ethyl (+)-(6R, 7R)-7-
[2-(2-amino-4-thiazolyl)-2-[(Z) methoxyimino] acetamido]-3-
methoxy methyl- 8-oxo-5-thia-1-azabicyclo [4.2.0] oct-2-ene-2-
carboxylate. The molecular formula of cefpodoxime proxetil 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.
Bromothymol blue C27H28Br2O5S (BTB), acts as a weak acid in
solution. It can thus be in protonated or deprotonated form,
appearing yellow or blue, respectively. It is bluish green in neutral
solution. The deprotonating of the neutral form results in a highly
conjugated structure, accounting for the difference in color. An
intermediate of the deprotonating mechanism is responsible for the
greenish color in neutral solution, mol. mass 624.38 g [4], see
scheme 2. Bromothymol blue has been used as a reagent to form ion
pair complexes with drugs as diltiazem HCl [5].
Scheme 1: Chemical structure of cefpodoxime proxetil (CEFP)
Scheme 2: Chemical structure of bromothymol blue
(C27H28Br2O5S)
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 bromocresol purple
and bromocresol green, receptively, in acidic medium and the
subsequent extraction of the ion-pair in chloroform [6].
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. In this case, the extracted complexes were into an
organic solvent, which is immiscible with water, and the
concentration of the resulting complex in the organic phase is
determined spectrophotometrically. 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 methods reported in the literature is based on the
formation of a complex between BTB and CEFP.
International Journal of Pharmacy and Pharmaceutical Sciences
ISSN- 0975-1491 Vol 8, Issue 8, 2016