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Stress Degradation Studies and HPLC Method Development for Simultaneous Estimation of Prednisolone Acetate and Chloramphenicol in Topical Eye Drops
Corresponding Author(s) : M. Ahsan Hafiz
Asian Journal of Chemistry,
Vol. 26 No. 22 (2014): Vol 26 Issue 22
Abstract
A rapid reversed phase liquid chromatographic method was developed and validated for simultaneous HPLC determination of chloramphenicol and prednisolone acetate. The proposed method was effectively applied on separation of chloramphenicol and prednisolone acetate in the presence of excipients and degradation products in eye drops. Chromatographic separation was achieved using combination of ammonium acetate buffer (0.02 M; pH 4) and methanol (30:70 v/v) at a flow rate of 1.5 mL/min. The effluent from column was monitored at 276 and 245 nm for chloramphenicol and prednisolone acetate, respectively. A good linear relationship was observed over the concentration ranges 0.0256-80 and 0.064-200 μg/mL with correlation coefficient 0.9999 and 0.9999 for chloramphenicol and prednisolone acetate, respectively. Calculated LOQ were 36 ng/mL for chloramphenicol and 31 ng/mL for prednisolone acetate. Active ingredients (chloramphenicol and prednisolone acetate) and degradation products were resolved in less than 4 min. The developed method was validated according to ICH guidelines.
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- J.M.L. Gallego and J.P. Arroyo, J. Pharm. Biomed. Anal., 31, 873 (2003); doi:10.1016/S0731-7085(02)00666-0.
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- H. Ashwin, S. Stead, J. Taylor, J. Startin, S. Richmond, V. Homer, T. Bigwood and M. Sharman, Anal. Chim. Acta, 529, 103 (2005); doi:10.1016/j.aca.2004.08.035.
- S.G. Musharraf, U. Fatima and R. Sultana, Chem. Cent. J., 6, 9 (2012); doi:10.1186/1752-153X-6-9.
- H.T. Rønning, K. Einarsen and T.N. Asp, J. Chromatogr. A, 1118, 226 (2006); doi:10.1016/j.chroma.2006.03.099.
- M.E. Falagas, A.P. Grammatikos and A. Michalopoulos, Expert Rev. Anti Infect. Ther., 6, 593 (2008); doi:10.1586/14787210.6.5.593.
- Y. Hongxin, Chinese Pharm. Affairs, 6, 410 (2007).
- P. Katakam and K. Sireesha, Asian J. Pharm. Clin. Res., 5, 182 (2012).
- D.A. Armbruster, M.D. Tillman and L.M. Hubbs, Clin. Chem., 40, 1233 (1994).
- ICH Q2 (R1) Validation of analytical procedures: text and methodology.http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q2_R1/Step4/Q2_R1__Guideline.pdf (Accessed on 15 March 2014).
- ICH Harmonised tripartite guideline, Validation of analytical procedures: Methodology. http://www.hc-sc.gc.ca/dhp-mps/alt_formats/hpfb-dgpsa/pdf/prodpharma/q2b-eng.pdf (Accessed on 02 March 2014).
References
J.M.L. Gallego and J.P. Arroyo, J. Pharm. Biomed. Anal., 31, 873 (2003); doi:10.1016/S0731-7085(02)00666-0.
S.N. Razzaq, I.U. Khan, I. Mariam and S.S. Razzaq, Chem. Cent. J., 6, 94 (2012); doi:10.1186/1752-153X-6-94.
M. Diestelhorst, F. Aspacher, W. Konen, G. Krieglstein and R.D. Hilgers, Graef. Arch. Clin. Exp, 230, 451 (1992); doi:10.1007/BF00175932.
L. Valvo, A. Paris, A. Savella, B. Gallinella and E.C. Signoretti, J. Pharm. Biomed. Anal., 12, 805 (1994); doi:10.1016/0731-7085(93)E0029-M.
S. Ahmed and M. Riaz, Chromatographia, 31, 67 (1991); doi:10.1007/BF02290499.
H. Ashwin, S. Stead, J. Taylor, J. Startin, S. Richmond, V. Homer, T. Bigwood and M. Sharman, Anal. Chim. Acta, 529, 103 (2005); doi:10.1016/j.aca.2004.08.035.
S.G. Musharraf, U. Fatima and R. Sultana, Chem. Cent. J., 6, 9 (2012); doi:10.1186/1752-153X-6-9.
H.T. Rønning, K. Einarsen and T.N. Asp, J. Chromatogr. A, 1118, 226 (2006); doi:10.1016/j.chroma.2006.03.099.
M.E. Falagas, A.P. Grammatikos and A. Michalopoulos, Expert Rev. Anti Infect. Ther., 6, 593 (2008); doi:10.1586/14787210.6.5.593.
Y. Hongxin, Chinese Pharm. Affairs, 6, 410 (2007).
P. Katakam and K. Sireesha, Asian J. Pharm. Clin. Res., 5, 182 (2012).
D.A. Armbruster, M.D. Tillman and L.M. Hubbs, Clin. Chem., 40, 1233 (1994).
ICH Q2 (R1) Validation of analytical procedures: text and methodology.http://www.ich.org/fileadmin/Public_Web_Site/ICH_Products/Guidelines/Quality/Q2_R1/Step4/Q2_R1__Guideline.pdf (Accessed on 15 March 2014).
ICH Harmonised tripartite guideline, Validation of analytical procedures: Methodology. http://www.hc-sc.gc.ca/dhp-mps/alt_formats/hpfb-dgpsa/pdf/prodpharma/q2b-eng.pdf (Accessed on 02 March 2014).