Development and Validation of a Stability-Indicating HPTLC Method for Analysis of Rasagiline Mesylate in the Bulk Drug and Tablet Dosage Form

A simple and sensitive thin-layer chromatographic method has been established for analysis of rasagiline mesylate in pharmaceutical dosage form. Chromatography on silica gel 60？F254 plates with 6？:？1？:？2(v/v/v) butanol-methanol water as mobile phase furnished compact spots at ？？ . Densitometric analysis was performed at 254？nm. To show the specificity of the method, rasagiline mesylate was subjected to acid, base, neutral hydrolysis, oxidation, photolysis, and thermal decomposition, and the peaks of degradation products were well resolved from that of the pure drug. Linear regression analysis revealed a good linear relationship between peak area and amount of rasagiline mesylate in the range of 100–350？ng/band. The minimum amount of rasagiline mesylate that could be authentically detected and quantified was 11.12 and 37.21？ng/band, respectively. The method was validated, in accordance with ICH guidelines for precision, accuracy, and robustness. Since the method could effectively separate the drug from its degradation products, it can be regarded as stability indicating. 1. Introduction Rasagiline mesylate (Figure 1) is a chemical inhibitor of the enzyme monoamine oxidase type-B which has a major role in the inactivation of biogenic and diet-derived amines in the central nervous system. Rasagiline is a propargylamine-based drug indicated for the treatment of idiopathic Parkinson’s disease. It is designated chemically as (R)-N-(prop-2-ynyl)-2,3-dihydro-1H-inden-1-amine. Rasagiline is freely soluble in water and ethanol and sparingly soluble in isopropyl alcohol. It is a chiral compound with one asymmetric carbon atom in a five-member ring with an absolute R-configuration which is produced as single enantiomer [1]. Figure 1: Structure of rasagiline mesylate. There are many methods reported in the literature for analysis of rasagiline mesylate, for example, GC-MS [2], HPLC methods [3–5], LC-MS/MS in human plasma [6], and spectrophotometric methods [7, 8]. However, no available densitometric method for the simultaneous separation of rasagiline mesylate from degradation products has been reported. Hence, the objective of the present study is to develop and validate a new HPTLC method for the estimation of rasagiline mesylate in bulk drug and its dosage form. Today, HPTLC is rapidly becoming a routine analytical technique due to its advantages of low operating costs high sample throughput, and need for minimum sample preparation. The major advantage of HPTLC is that several samples can be run simultaneously using a small quantity of mobile phase unlike HPLC,