Development and Validation of Stability Indicating HPTLC Method for Determination of Diacerein and Aceclofenac as Bulk Drug and in Tablet Dosage Form

S P Gandhi,T C Borole,M C Damle,M G Dewani

doi:10.1155/2012/719264

Abstract

Diacerein is a drug for osteoarthritis and is di-acetylated derivative of rein. Aceclofenac is used as an effective non-steroidal anti-inflammatory drug (NSAID) with anti-inflammatory, analgesic, and antipyretic properties. The present study describes degradation of diacerein and aceclofenac under ICH prescribed stress conditions (hydrolysis, oxidation, dry heat, wet heat, and photolysis) and establishment of a stability-indicating HPTLC assay method. Different degradation peaks were observed for diacerein when it was exposed to alkaline, and acid catalysed hydrolysis. For aceclofenac, decrease in peak area was observed with single peak of degradation product after oxidation. For HPTLC, RP-18 F254spre-coated plates, and mobile phase consisting of methanol: water 7: 3 v/v was used to achieve separation. Quantitation was done at 268 nm. The method was validated as per ICH Q2 R1 guidelines and results were in limit. The method was found to be simple, specific, precise, and stability indicating.

Highlights

Diacerein 4,5-bis(acetoxy)-9,10-dihydro-9,10-dioxo-2-anthracenecarboxylic acid is drug for osteoarthritis[1,2]
This paper describes a simple, accurate, sensitive, and validated stability indicating HPTLC method for diacerein and aceclofenac in combination as the bulk drug and in tablet dosage forms as per ICH guidelines[17,18]
While no degradation peak was observed for aceclofenac with 88.95% recovery. [Figure 2] After acid hydrolysis, 62.48% Diacerein was recovered with 3 peaks (D1-D3) of degraded product while 41.75% Aceclofenac was recovered with no peak of degraded product [Figure 3]

Summary

Introduction

Diacerein 4,5-bis(acetoxy)-9,10-dihydro-9,10-dioxo-2-anthracenecarboxylic acid is drug for osteoarthritis[1,2]. This paper describes a simple, accurate, sensitive, and validated stability indicating HPTLC method for diacerein and aceclofenac in combination as the bulk drug and in tablet dosage forms as per ICH guidelines[17,18]. Standard stock solution of Diacerein and aceclofenac were prepared separately by dissolving 25 mg of drug in 25 mL of methanol to get concentration of 1000 mcg/mL. 2.5 mL of mixed working standard solution of diacerein was mixed with 2.5 mL of 0.1 N HCl. The solution was diluted to 25 mL with methanol and kept for 15 min. Photolytic studies were carried out by exposure of drug as mixture to UV light up to 200 watt hours/square meter and subsequently to cool fluorescent light to achieve an illumination of 1.2 million Lux.Hr. Samples were weighed, dissolved and diluted get 10 μg/mL

Method Validation

Results and Discussion

Conclusion