QUANTIFICATION OF PYRITINOL IN SOLID PHARMACEUTICAL FORMULATION BY HIGH-PERFORMANCE THIN-LAYER CHROMATOGRAPHY-ULTRAVIOLET DETECTION AND SELECTIVITY EVALUATION BY MASS SPECTROMETRY

摘要

A high-throughput method for pyrilinol quantification in solid pharmaceutical formulation was developed. Chromalography was performed on silica gel 6OF_(254) HPTLC plates using the mixture dichloromelhane - melhanol -formic acid 9:1:1 (v/v/v) as mobile phase. Detection was carried out by UV absorbance at 300 nm. Calibration showed a polynomial regression with a determination coefficient (R2) of 0.9992. For chromalography, repeatability (relative standard deviation, RSD) and intermediate precision (RSD) in matrix were 0.4% and 3. 0%, respectively. Recoveries of spiked, samples at three levels ranging from 98.5 to 101. 9% with intermediate precisions of RSD 3.7 to 4.7%. Limits of detection and quantification were 0.6 and 2.0 mug mL~(-1) (6 and 20 ng/band), respectively. The method capacity to deled degradation products and/ or byproducts within routine conditions of analysis was evaluated through forced degradation processes. Selectivity was evaluated determining the peak purity by UV-speclropholomehy, which showed, coirelalion coefficients (r) > 0.9997. Additionally, peak identity and purity was confirmed by mass speclromelry. The mass spectra showed just pyritinol ions at m/z 369 [M+H]~+ and 391 [M+Na]~+ being acquired directly from the sample bands by an elulion-based interface. Considering the validation results, reduced analysis cost, accelerated analysis time, and high throughput capacity, this simple, yet reliable planar chromatographic method is a good alternative for pyritinol analysis in pharmaceutical fonnulations.