Advertisement

Chromatographia

, Volume 64, Issue 1–2, pp 95–100 | Cite as

Development and Validation of a LC Method for the Determination of Pramipexole Using an Experimental Design

  • G. Srinubabu
  • K. Jaganbabu
  • B. Sudharani
  • K. Venugopal
  • G. Girizasankar
  • J. V. L. N. S. Rao
Article

Abstract

A rapid and sensitive RP-HPLC method with UV detection for routine control of pramipexole in tablets was developed. Chromatography was performed with mobile phase containing a mixture of acetonitrile/phosphate buffer (60/40; v/v) with a flow rate of 0.8 mL min−1. Quantitation was accomplished with the internal standard method; the procedure was validated by linearity (correlation coefficient = 0.99892), accuracy, robustness and intermediate precision. Limit of quantitation and limit of detection were found to be 4.5 µg and 1.4 µg respectively, which indicates the method is highly sensitive. Experimental design was used during validation to calculate method robustness and intermediate precision, for robustness test three factors were considered; percentage v/v of acetonitrile, flow rate and pH; an increase in the flow rate results in a decrease of concentration found of the drug, while the percentage of organic modifier and temperature have no important effect on the response. For intermediate precision measure the considered variables were: analyst, equipment, days and obtained RSD value (0.56%, n=24) which indicated a good precision of the analytical method. The method was found to be applicable for determination of the drug in tablet formulations and the results of the developed method were compared with those of the UV spectrophotometric method to access the active pramipexole content.

Keywords

Column liquid chromatography UV spectrophotometry Robustness testing Experimental design Pramipexole 

Preview

Unable to display preview. Download preview PDF.

Unable to display preview. Download preview PDF.

References

  1. Ling ZD, Robbie HC, Tong CW, Carve PM (1999) J Pharmacol Exp Ther 289:202–210Google Scholar
  2. Ramirez AD, Wong SK, Menniti FS (2003) Eur J Pharmacol 475:29–35CrossRefGoogle Scholar
  3. Pan T, Xie W, Jankovic J, Le W (2005) Neurosci Lett 377:106–109CrossRefGoogle Scholar
  4. Gu M, Irvani M, Cooper JM, King D, Jenner P, Schapira AH (2004) J Neurochem 91:1075–1081CrossRefGoogle Scholar
  5. Ross MF, Kelso GF, Blaikie FH, James AM, Cocheme HM, Filipovska A, Da Ros T, Hurd TR, Smith RA, Murphy MP (2005) Biochemistry 70:222–230Google Scholar
  6. Andersen JK (2004) Nat Med 10 (Supp. l): 18–25Google Scholar
  7. Lau YY, Selenka JM, Hanson GD, Talaat R, Ichhpurani N (1996) J Chromatogr B Biomed Sciec Appl 683(2): 209–216CrossRefGoogle Scholar
  8. International Conference on Harmonisation, Topic Q2B, Validation of Analytical Methods: Methodology. The Third International Conference on Harmonisation of Technical Requirements for Registration of Pharmaceuticals for Human Use, (ICH) Yokohama, Japan, 29 November–1 December, 1996Google Scholar
  9. Molnar I (2005) Chromatogrphia. Vol 62 (suppl 13) pages s7 – s17Google Scholar
  10. Lin DK (1999) J Quality Technol 31:61–66Google Scholar
  11. Statistica software 2300 East 14th street, Tulsa, Ok 74104, USAGoogle Scholar
  12. Hockman KK, Berengut D (1995) Chem. Eng 102:142–148Google Scholar
  13. Fabre H (1996), J Pharm Biomed Anal 14:1125–1132Google Scholar
  14. Ragonese R, Mulholland M, Kalman J (2000) J Chromatogr A 870:45–51CrossRefGoogle Scholar
  15. Lewis GA, Mathieu D, Phan-Tan-Luu R (1999) Pharmaceutical Experimental Design, Marcel Dekker, New YorkGoogle Scholar
  16. Pinzauti S, Gratteri P, Furlanetto S, Mura P, Dreassi E, Phan-Tan-Luu RL J Pharm Biomed Anal 14:(1996) 881–889Google Scholar
  17. Ermer J, Ploss HJ (2005) J Pharm Biomed Anal 37:859–870CrossRefGoogle Scholar
  18. Srinubabu G, Raju ChAI Asain. J. Chem vol. 18 issue 4 (in press)Google Scholar

Copyright information

© Friedr. Vieweg & Sohn/GWV Fachverlage GmbH 2006

Authors and Affiliations

  • G. Srinubabu
    • 1
    • 3
  • K. Jaganbabu
    • 2
  • B. Sudharani
    • 1
  • K. Venugopal
    • 1
  • G. Girizasankar
    • 2
  • J. V. L. N. S. Rao
    • 1
  1. 1.Department of Pharmaceutical SciencesCollege of Engineering, Andhra UniversityVisakhapatnamIndia
  2. 2.Shri Vishnu College of PharmacyBhimavaramIndia
  3. 3.Center for Biotechnology, Department of Chemical EngineeringAndhra University, College of EngineeringVisakhapatnamIndia

Personalised recommendations