Development and Validation of Chiral HPLC Method for Quantification of 3-(S)-Quinuclidinol in Pharmaceutically Important Precursor, 3-(R)-Quinuclidinol, by Precolumn Derivatization
| Autor: | Ravindra B. Shinde, Santosh K. Gaykar, Jayvant Harlikar, Srinivas V. Pullela, Manish Gangrade, Chetan M. Bhalgat |
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| Rok vydání: | 2016 |
| Předmět: |
Diethylamine
Active ingredient Detection limit Chromatography Resolution (mass spectrometry) 010405 organic chemistry 010401 analytical chemistry General Medicine Repeatability 01 natural sciences High-performance liquid chromatography 0104 chemical sciences Analytical Chemistry Chiral column chromatography chemistry.chemical_compound chemistry Phase (matter) |
| Zdroj: | Journal of chromatographic science. 54(10) |
| ISSN: | 1945-239X |
| Popis: | A sensitive and specific high-performance liquid chromatography (HPLC) method for the separation and quantification of 3-(S)-quinuclidinol in 3-(R)-quinuclidinol, precursor for active pharmaceutical ingredients (solifenacin, revatropate and talsaclidine), has been developed and validated by precolumn derivatization. Several chiral columns were tested in a normal phase system. Excellent enantioseparation with the resolution more than 11.4 was achieved on Chiralpak IC column using isocratic mobile phase consisting of n-hexane, ethanol, 2-propanol and diethylamine (80:8:12:0.4, v/v). The detection was carried out using UV detector at 230 nm. The influence of mobile phase composition, namely organic modifiers, additives, aliphatic alkanes and water content in mobile phase, on retention and enantioseparation was studied. Validation of the developed method including specificity, system suitability, limit of detection, limit of quantification, linearity, repeatability, intermediate precision, accuracy and solution stability was performed according to the International Conference on Harmonization guidelines. The advantage of the method is a good HPLC enantioseparation by precolumn derivatization using reaction mixture as sample, simpler UV detection, short analysis time ( |
| Databáze: | OpenAIRE |
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