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.
Highlights
Impurity profiling of active pharmaceutical ingredients and formulations is one of the most challenging tasks of analytical chemists in the pharmaceutical industry [1]
Stress studies were performed at an initial concentration of 1000 μg/mL of TOLP in the active pharmaceutical ingredients (API) and formulated the sample to provide the stability-indicating property and specificity of the proposed method
Intentional degradation was attempted by the stress conditions of photolytic, heat, acid (0.1N HCl refluxed for 1 hr at 60°C), base (0.1N NaOH refluxed for 45min at 60°C), oxidation (8%H2O2 refluxed for 45 min at 60°C), water, and humidity
Summary
Impurity profiling of active pharmaceutical ingredients and formulations is one of the most challenging tasks of analytical chemists in the pharmaceutical industry [1]. The presence of unwanted or in certain cases unknown chemicals, even in small amounts, may influence the therapeutic efficacy and the safety of the pharmaceutical products [2] For these reasons, all major international pharmacopoeias have established maximum allowed limits for related compounds for both bulk and formulated APIs. As per the requirements of various regulatory authorities, the impurity profile study of drug substances and drug products has to be carried out using a suitable analytical method in the final product [3, 4]. An attempt has been made to develop an accurate, rapid, specific, and reproducible method for the determination of TOLP impurities in bulk drug samples and in pharmaceutical dosage forms along with method validation as per ICH norms [18, 19].
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