STABILITY INDICATING ANALYTICAL METHOD DEVELOPMENT AND VALIDATION OF HPLC FOR PREGABALIN QUANTIFICATION IN BULK AND PHARMACEUTICAL DOSAGE FORMULATIONS

Authors : Kenan Can Tok
Pages : 45-57
Doi:10.33483/jfpau.1681060
View : 138 | Download : 336
Publication Date : 2026-01-13
Article Type : Research Paper
Abstract :Objective: To develop and validate a rapid, sensitive, and cost-effective HPLC-UV method for the quantification of pregabalin (PRG) in both bulk drug substance and pharmaceutical dosage formulations, addressing the growing need for robust analytical techniques in pharmaceutical quality control and forensic toxicology. Material and Method: An HPLC-UV method was developed using an Agilent 1100/1200 system equipped with a UV detector and a Merck monolithic silica column (100 mm x 4.6 mm). The mobile phase consisted of acetonitrile and water (5:95, v/v) adjusted to pH 7.0 with orthophosphoric acid and sodium hydroxide, at a flow rate of 2.0 ml/min and a column temperature of 45°C. UV detection was set at 200 nm. The method was validated according to ICH Q2(R1) guidelines, evaluating linearity, sensitivity, accuracy, precision, recovery, and stability-indicating properties through forced degradation studies. Result and Discussion: The developed HPLC-UV method demonstrated rapid analysis with a pregabalin retention time of 1.44 minutes and a total run time under 2 minutes. System suitability parameters met pharmacopeial requirements. The method exhibited excellent linearity in the range of 1 to 150 µg/ml (R² > 0.999), with LOD and LOQ values of 0.25 µg/ml and 0.76 µg/ml, respectively. Intra-day and inter-day accuracy ranged from 96.09% to 99.68% and 95.07% to 98.78%, respectively, with RSD values for precision consistently below 2.22%. Recovery from pharmaceutical formulations was between 99.0% and 101.75%. Forced degradation studies revealed that pregabalin is stable under acidic, oxidative, and thermal stress conditions, as well as during freeze-thaw and autosampler storage, but is susceptible to base hydrolysis. The validated HPLC-UV method is demonstrated to be rapid, accurate, precise, and stability-indicating, making it suitable for routine quality control of pregabalin in pharmaceutical products and for forensic applications.
Keywords : Adli eczacılık, adli toksikoloji, HPLC-UV, metot geliştirme ve geçerli kılma, pregabalin

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