Validation of HPLC methods for analyzing the chemical purity of cilostazol

Magdalena Kossykowska 1Marta Zezula 1Justyna Chmiel 1Marta Jatczak 1Anna Ostaszewska 2Joanna Zagrodzka 1Katarzyna Badowska-Rosłonek 1

1. Pharmaceutical Research Institute (IF), Rydygiera 8, Warszawa 01-793, Poland
2. Instytut Farmaceutyczny (PRI), Rydygiera 8, Warszawa 01-793, Poland

Abstract

Two selective HPLC methods with UV detection were developed to analyse cilostazol and its related substances. Due to great difference between spectral properties of the analytes,  the analysis was divided into two independent parts. Separation of cilostazol and its potential impurities was achieved on Kinetex C18 chromatographic column (100 mm x 4.6 mm x 2.6 μm) by gradient elution with ammonium acetate buffer and acetonitrile. Chromatograms were acquired at 254 nm. The second method for the quantitative determination of CX-1 (starting material in the synthetic route) assay was investigated on Synergi MAX-RP chromatographic column (150 mm x 4.6 mm x 4 μm) with the use of H2O:CH3CN (1:1, v/v) mixture and isocratic elution. Detection was carried out at 193 nm.

Both methods were validated for linearity, specificity, precision, accuracy, limit of detection, limit of quantification and robustness. Suitability of HPLC methods for the pharmaceutical control of cilostazol samples and the validation according to requirements of Q2(R1) International Conference of Harmonization scientific guideline were demonstrated.

Acknowledgement:

Research Project has been supported by European Union (under European Regional Development Fund) No. UDA-POIG.01.03.01-14-062/09-00 “Innovative technologies of cardiovascular medicines of special therapeutic and social importance”

 

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Presentation: Poster at IX Multidyscyplinarna Konferencja Nauki o Leku, by Magdalena Kossykowska
See On-line Journal of IX Multidyscyplinarna Konferencja Nauki o Leku

Submitted: 2014-03-13 08:40
Revised:   2014-05-05 16:08