Optimization of chromatographic systems for detection and determination of carbamazepine in pharmaceutical formulations, serum, and saliva by HPLC-DAD

Abstract

Carbamazepine (CBZ) is an anticonvulsant drug, widely used also in various disorders like neuropathic pain, bipolar affective disorder, resistant schizophrenia, and trigeminal neuralgia. Appropriate analytical procedures are necessary to monitor, detect and quantify CBZ in pharmaceutical formulations and biological samples. The search for new methods for drug determination is one of the most important challenges of modern scientific research. It is important to study the chromatographic conditions of CBZ analysis, which is necessary for the further development of efficient drug determination methods. In this work, retention, peak symmetry, and system efficiency of CBZ on Polar RP and Phenyl-Hexyl stationary phases were investigated. Various mobile phases containing methanol (MeOH) and/or acetonitrile (ACN) as organic modifiers, acetate buffer, and the addition of diethylamine (DEA) were applied. Different chromatographic systems were compared to obtain satisfying retention, peak shape, and system efficiency. The most optimal chromatographic system with Polar RP column was applied for the determination of CBZ in pharmaceutical formulations, human serum, and saliva by the high-performance liquid chromatography with diode array detection (HPLC-DAD) method. Solid-phase extraction (SPE) method was applied for sample preparation prior to chromatographic analysis. The proposed method was validated for linearity, selectivity, precision, and accuracy. Confirmation of the presence of CBZ and its main metabolites in biological samples obtained from patients was performed using the ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method.