Journalartikel

Jahr der Veröffentlichung: 2010

Seiten: 957-971

Zeitschrift: Journal of Liquid Chromatography and Related Technologies

Bandnummer: 33

Heftnummer: 7-8

DOI Link: https://doi.org/10.1080/10826071003766062

Verlag: Taylor and Francis Group

Abstract: 

A high-throughput method for pyritinol quantification in solid pharmaceutical formulation was developed. Chromatography was performed on silica gel 60F254 HPTLC plates using the mixture dichloromethane - methanol - formic acid 9:1:1 (v/v/v) as mobile phase. Detection was carried out by UV absorbance at 300nm. Calibration showed a polynomial regression with a determination coefficient (R2) of 0.9992. For chromatography, 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 2.0g mL-1 (6 and 20ng/band), respectively. The method capacity to detect 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-spectrophotometry, which showed correlation coefficients (r)0.9997. Additionally, peak identity and purity was confirmed by mass spectrometry. 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 elution-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 formulations.

Harvard-Zitierstil: Aranda, M. and Morlock, G. (2010) Quantification of pyritinol in solid pharmaceutical formulation by high-performance thin-layer chromatography-ultraviolet detection and selectivity evaluation by mass spectrometry, Journal of Liquid Chromatography and Related Technologies, 33(7-8), pp. 957-971. https://doi.org/10.1080/10826071003766062

APA-Zitierstil: Aranda, M., & Morlock, G. (2010). Quantification of pyritinol in solid pharmaceutical formulation by high-performance thin-layer chromatography-ultraviolet detection and selectivity evaluation by mass spectrometry. Journal of Liquid Chromatography and Related Technologies. 33(7-8), 957-971. https://doi.org/10.1080/10826071003766062