Abstract
A new and accurate chiral liquid chromatographic method has been developed for the determination of enantiomeric purity of darifenacin [(S)-enantiomer] in bulk drugs and extended release tablets. Normal phase chromatographic separation was performed on an immobilized cellulose based chiral stationary phase (Chiralpak-IC) with n-hexane:ethanol:diethylamine (50:50:0.3, v/v/v) as mobile phase at a flow rate of 1.0 mL min−1. The elution time was ~15 min. The resolution (R s ) between the enantiomers was greater than four and interestingly the (R)-enantiomer was eluted prior to darifenacin in the developed method. The limit of detection (LOD) and limit of quantification (LOQ) for the (R)-enantiomer were 0.02 μg and 0.07 μg, respectively, for a 10 μL injection volume. The method was extensively validated in terms of linearity, precision and accuracy and satisfactory results were obtained. Robustness studies were also conducted. The sample solution stability of darifenacin was determined and the compound was found to be stable for a study period of 48 h.
Similar content being viewed by others
References
Wallis RM, Burges RA, Cross PE, Mackenzie AR, Newgreen DT, Quinn P (1995) Pharmacol Res 31:54. doi:10.1016/1043-6618(95)86474-1
Michel MC, Oelke M, Zinner N (2005) Drug Discov Today Ther Strateg 2:1–6
Chancellor M, Aronstein WS, Egermark M, Ariely R, Ebinger U, Kianifard F (2007) Urology 70:88. doi:10.1016/j.urology.2007.06.368
Foote J, Glavind K, Kralidis G, Wyndale J-J (2005) Eur Urol 48:471–477
Wang P, Luthin GR, Ruggieri MR (1995) J Pharmacol Exp Ther 273:959
Sahajwalla CG (2004) New drug development, vol 141. Marcel Dekker Inc., New York, pp 421–426
Beesley TE, Scott RPW (1998) Chiral Chromatography. Wiley, New york, pp 23–26
Subramanian G (1994) A practical approach to chiral separations by liquid chromatography. VCH Publishers, Weinheim
Aboul-Enein HY, Wainer IW (1997) The impact of stereochemistry in drug development and use. Wiley, New York
Allenmark S (1991) Chromatographic enantioseparation: methods and applications, 2nd edn. Ellis Horwood, New York
Kaye B, Herron WJ, Macrae PV, Robinson S, Stopher DA, Venn RF et al (1996) Anal Chem 68:1658–1660. doi:10.1021/ac9507552
Zhang T, Nguyen D, Franco P, Isobe Y, Michishita T, Murakami T (2008) J Pharm Biomed Anal 46:882–891. doi:10.1016/j.jpba.2007.06.008
Draft ICH Guidelines on Validation of Analytical Procedures (1995) Definitions and terminology. Federal Register, vol 60. IFPMA, Switzerland, p 11260
Validation of compendial methods (2007) The United States pharmacopeia, 30th edn. USP30
Author information
Authors and Affiliations
Corresponding author
Rights and permissions
About this article
Cite this article
Radhakrishnanand, P., Subba Rao, D.V. & Himabindu, V. A Validated LC Method for Determination of the Enantiomeric Purity of Darifenacin in Bulk Drug and Extended Release Tablets. Chroma 68, 1059–1062 (2008). https://doi.org/10.1365/s10337-008-0795-z
Received:
Revised:
Accepted:
Published:
Issue Date:
DOI: https://doi.org/10.1365/s10337-008-0795-z