title: Development and Validation of a Precise, Single HPLC Method for the Determination of Tolperisone Impurities in API and Pharmaceutical Dosage Forms.
abstract: A novel, sensitive, stability-indicating HPLC method has been developed for the quantitative estimation of Tolperisone-related impurities in both bulk drugs and pharmaceutical dosage forms. Effective chromatographic separation was achieved on a C18 stationary phase with a simple mobile phase combination delivered in a simple gradient programme, and quantitation was by ultraviolet detection at 254 nm. The mobile phase consisted of a buffer and acetonitrile delivered at a flow rate 1.0 ml/min. The buffer consisted of 0.01 M potassium dihydrogen phosphate with the pH adjusted to 8.0 by using diethylamine. In the developed HPLC method, the resolution between Tolperisone and its four potential impurities was found to be greater than 2.0. Regression analysis showed an R value (correlation coefficient) of greater than 0.999 for the Tolperisone impurities. This method was capable of detecting all four impurities of Tolperisone at a level of 0.19 μg/mL with respect to the test concentration of 1000 μg/mL for a 10 µl injection volume. The tablets were subjected to the stress conditions of hydrolysis, oxidation, photolysis, and thermal degradation. Considerable degradation was found to occur in base hydrolysis, water hydrolysis, and oxidation. The stress samples were assayed against a qualified reference standard and the mass balance was found to be close to 100%. The established method was validated and found to be linear, accurate, precise, specific, robust, and rugged.
authors: Analytical Research and Development, Integrated Product Development, Dr. Reddy's Laboratories Ltd., Bachupally, Hyderabad-500072, India.
authors: Thummala Veera Raghava
authors: TV
authors: Raju
authors: Raja Kumar
authors: RK
authors: Seshadri
authors: Srinivas
authors: S
authors: Arutla
authors: Tharlapu Satya Sankarsana Jagan
authors: TS
authors: Mohan
authors: Ivaturi Mrutyunjaya
authors: IM
authors: Rao
authors: Someswara Rao
authors: SR
authors: Nittala
keywords: Degradation; HPLC; Impurities; Tolperisone; Validation
references: J Pharm Biomed Anal. 1999 Jun;20(1-2):401-4
references: 10704049
references: Eur J Pharmacol. 2006 May 24;538(1-3):5-14
references: 16650844
references: Arch Pharm Res. 2006 Apr;29(4):339-42
references: 16681042
references: J Pharm Biomed Anal. 2001 Dec;26(5-6):865-72
references: 11600298
references: Joint Bone Spine. 2007 Jan;74(1):e1-8
references: 17218139
references: J Pharmacol Exp Ther. 2005 Dec;315(3):1237-46
references: 16126840