Журнал хроматографии и методов разделения
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Application of a Validated Stability-Indicating HPTLC Method for Simultaneous Estimation of Paracetamol and Aceclofenac and their Impurities

Archana Ambekar

A sensitive, accurate, precise and stability indicating HPTLC method has been developed and validated for the simultaneous determination of Paracetamol (PCT), Aceclofenac (ACF) and their impurities namely, 4-amino phenol (AP) and Diclofenac acid (DA), respectively, which are the hydrolytic degradation products and related substances of the drugs. The chromatographic separation was achieved using optimized mobile phase, ethyl acetate: methanol: glacial acetic acid (8.5:1.5:0.25 V/V) on pre-activated silica gel 60 F254 TLC plates with ultraviolet detection at 231 nm. Statistical analysis revealed linear relationships in the concentration ranges of 3900–9100, 1200–2800 for PCT, ACF respectively and 100-600 ng/band for AP and DA with correlation coefficient more than 0.99. The chromatographic conditions gave compact spots at Rf value (± SD) 0.60 (± 0.011), 0.21 (± 0.01), 0.83 (± 0.01) and 0.08 (± 0.015) for PCT, ACF, AP and DA respectively. The method was validated as per ICH guidelines, demonstrating to be accurate and precise within the corresponding linearity range of analytes. Inherent stability of these drugs was studied by exposing drug substances to stress conditions as per ICH guidelines namely oxidative, thermal, photolysis and hydrolytic conditions under different pH. Relevant degradation was found to take place under these conditions. PCT and ACF were found to undergo extensive acidic and basic hydrolysis while ACF was also susceptible to neutral hydrolysis; producing stated impurities as their major degradation products. The developed method resolved the drugs from degradation products generated under stress conditions; with the peak purity values greater than 0.999. Thus, a new simple, accurate, precise, sensitive and economic stability-indicating High Performance Thin Layer Chromatography (HPTLC)/densitometry method has been developed and validated for the simultaneous estimation of the titled analytes and their stated impurities in pharmaceutical dosage form. The high sensitivity and specificity make it valuable quantitative method suitable to be employed in the routine estimation of impurities and in stability studies.