A VALIDATED NEW GRADIENT STABILITY-INDICATING LC METHOD FOR THE SIMULTANEOUS ESTIMATION OF CILOSTAZOL AND ASPIRIN IN BULK AND TABLET FORMULATION
Archana M. Ambekar*, Dr. B. S. Kuchekar
ABSTRACT
A simple, precise and gradient RP-HPLC method was developed and
validated for the simultaneous estimation of Cilostazol (CIL) and
Aspirin (ASP) in presence of their corresponding degradation products.
The RP-HPLC method consisted of a Binary pumps (model Waters
515 HPLC pump) and auto sampler (model 717 plus) was used.
Chromatographic separation was achieved with Nova-pack C18
(4.6mm x 250 mm, particle size 4µm) column using gradient mode of
elution. The mobile phase comprises of Acetonitrile: Ammonium
formate (10 mm) pH 3.5 (adjusted with Ortho Phosphoric acid) in
gradient mode. The flow rate was 0.7 ml/min and column temperature maintained at 40ºC
throughout separation. The eluent was monitored at 254 nm using photodiode array detector
(Waters 2998). The retention times of CIL and ASP were 24.5 ± 0.33 min and 16.3 ± 0.19
min respectively. The method was validated in terms of specificity, accuracy, linearity,
precision, limit of detection, limit of quantitation and robustness. Linearity for CIL and ASP
was in the range of 5 to 100 µg/ml and 2 to 40 µg/ml, respectively and percentage recoveries
of both analytes were in the range of 100 1.5% and % RSD was <1.5. The stress testing of
both the drugs individually and combined was carried out under acidic, alkaline, neutral,
oxidation, photo-stability and dry heat conditions. ASP underwent extensive acid, base,
neutral hydrolysis and oxidative degradation than photo and thermal degradation. On the other hand, CIL was susceptible to acid, alkaline and oxidative degradation; while, it showed
stability towards neutral hydrolysis, photo and thermal degradation. The degradation products
were well resolved from the analyte peaks. Thus the proposed method was suitable for
quantitative determination and stability study of CIL and ASP in pharmaceutical preparations
and can be used in the quality control of bulk manufacturing and pharmaceutical dosage
forms.
Keywords: HPLC, Cilostazol, Aspirin, stability indicating method.
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