Original Article Rasagiline hemitartrate: Synthesis, characterization and RP-HPLC validation for its estimation in bulk form Muvvala S. Sudhir a,c , Ratnakaram Venkata Nadh b, * a Department of Chemistry, Sri Subbaraya and Narayana College, Narasaraopet 522 601, Andhra Pradesh, India b School of Biotechnology, Vignan University, Guntur 522213, India article info Article history: Received 9 January 2013 Accepted 14 May 2013 Keywords: Rasagiline hemitartrate Synthesis Characterization RP-HPLC method Validation abstract Objectives: To develop a reverse phase high performance liquid chromatographic method for validation and quantitative estimation of the synthesized drug rasagiline hemitartrate in bulk form. Methods: Rasagiline hemitartrate was synthesized and characterized by spectral (Infrared, Proton Nuclear Magnetic Resonance and Mass) as well as elemental analysis. Chromato- graphic separation was conducted on Agilent TC-C18 (250  4.6 mm, 5 mm) column at ambient temperature using mixture of 20 mM potassium dihydrogen orthophosphate buffer (pH 7.0): methanol and acetonitrile in the ratio (30:30:40 v/v) as a mobile phase and at a flow rate of 1.0 mL/min, while UV detection was performed at 285 nm. In addition to LOD and LOQ, other analytical parameters viz., linearity, precision, accuracy, ruggedness and robustness were detected by following the ICH (International Conference on Harmonization) guidelines. Results: The retention time for rasagiline hemitartrate was found to be 4.30  0.05 min. The method was found to be linear in the range of 10e50 mg/mL. The limit of detection and quantization for rasagiline hemitartrate are found to be 0.651 and 1.972 mg/mL respectively. Analytical recovery was 100.47%. The percentage RSD for precision and accuracy of the method was found to be less than 2%. Correlation coefficient was found to be 0.9952. Conclusion: In this study, simple, sensitive, accurate and reliable RP-HPLC method was developed and validated as per the ICH guidelines for the determination of the synthesized drug rasagiline hemitartrate in bulk form. Copyright ª 2013, JPR Solutions; Published by Reed Elsevier India Pvt. Ltd. All rights reserved. 1. Introduction R(þ)-N-propargyl-1-aminoindan (rasagiline) is a chiral com- pound with one asymmetric carbon atom in a five member ring with an absolute with R-configuration which is produced as single enantiomer. 1 It is a propargylamine-based drug indicated for the treatment of idiopathic Parkinson’s disease. 2 In addition to rasagiline base, its acid addition salts (viz., mesylate, maleate, fumarate, tartrate, hydrobromide, esylate, p-tolunesulfonate, benzoate, acetate, phosphate and sulfate) are pharmaceutically acceptable. 3 Rasagiline was generally well tolerated in clinical trials as both monotherapy and when * Corresponding author. Tel.: þ91 9441027105. E-mail addresses: doctornadh@yahoo.co.in, doctornadh@gmail.com (R. Venkata Nadh). c Tel.: þ91 9490645147. Available online at www.sciencedirect.com journal homepage: www.elsevier.com/locate/dit drug invention today 5 (2013) 133 e138 0975-7619/$ e see front matter Copyright ª 2013, JPR Solutions; Published by Reed Elsevier India Pvt. Ltd. All rights reserved. http://dx.doi.org/10.1016/j.dit.2013.05.002