Optimization of hydrophilic interaction liquid chromatographic method for simultaneous determination of cetylpyridinium chloride and benzocaine in lozenges
DOI:
https://doi.org/10.20450/mjcce.2012.56Keywords:
benzocaine, cetylpyridinium chloride, HILIC, lozenges, retention mechanismAbstract
A new Hydrophilic Interaction Liquid Chromatography (HILIC) method was developed for simultaneous determination of cetylpyridinium chloride and benzocaine as active substances in lozenges. Method development included investigation of the influence of the critical chromatographic conditions such as: type of organic modifier, mobile phase strength, ionic strength and pH value of the buffer used in the mobile phase, as well as experimental determination of dominant mechanism of retention. The optimal chromatographic conditions were obtained using bare silica column and a mobile phase consisting of acetonitrile and ammonium formate (50 mM, pH = 4.0) in ratio 80 : 20 V/V. The method was validated in terms of specificity, linearity, accuracy and precision. The validation results indicate that the proposed HILIC method is suitable for quantitative analysis of cetylpyridinium chloride and benzocaine in lozenges.References
R. B. Taylor, S. Toasaksiri, R. G. Reid, D. Wood, Determination of the quaternary ammonium compounds dequalinium and cetylpyridinium chlorides in candy-based lozenges by high-performance liquid chromatography, Analyst. 122, 973–976 (1997).
Martindale the extra pharmacopoeia, Royal Pharmaceutical Society of Great Britain, London, England, 1996.
European Pharmacopeia 7.0, Council of Europe, Strasbourg, France, 2010.
M. Benamor, N. Aguersif, M.T. Draa, Spectrophotometric determination of cetylpyridinium chloride in pharmaceutical products, J. Pharm. Biomed. Anal. 26, 151–154 (2001).
L. J. Schep, D. S. Jones, I. Tucher, M. G. Shepherd, A colorimetric ion-pairing analytical method for quaternay ammonium compounds using eosin- Y and Triton X-100, Int. J. Pharm. 113, 263–266 (1995).
R. B. Taylоr, S. Toasaksiri, R. G. Reid, Determination of antibacterial quaternary ammonium compounds in lozenges by capillary electrophoresis, J. Chromatogr. A 798, 335–343 (1998).
L. M. Nair, R. Saari-Nordhaus, Recent developments in surfactant analysis by ion chromatography, J. Chromatogr. A 804, 233–239 (1998).
J. Wang, J. Lu, L. Zhang, Y. Hu, Determination of cetylpyridinium chloride and tetracaine hydrochloride in buccal tablets by RP-HPLC, J. Pharm. Biomed. Anal. 32, 381–386 (2003).
United States Pharmacopeia 31, United States Pharmacopeial Convention, Washington, 2008.
P. Linares, M. C. Gutierrez, F. Lazaro, M. D. Luque de Castro, M. Valcarcel, Determination of benzocaine, dextromethorphan and cetylpyridinium ion by high-performance liquid chromatography with UV-detection, J. Chromatogr. A 558, 147–153 (1991).
P. Hemström, K. Irgum, Hydrophilic interaction chromatography, J. Sep. Sci. 29, 1784–1821 (2006).
B. Dejaegher, Y. Vander Heyden, HILIC methods in pharmaceutical analysis, J. Sep. Sci. 33, 698–715 (2010).
L. Snyder, J. Kirkland, J. Dolan, Introduction to modern liquid chromatography, third ed., John Wiley & Sons Inc. : Hoboken, New Jersey, USA, 2010.
B. Dejaegher, D. Mangelings, Y. Vander Heyden, Method development for HILIC assays, J. Sep. Sci. 31, 1438–1448 (2008).
Z. Hao, B. Xiao, N. Weng, Impact of column temperature and mobile phase components on selectivity of HILIC, J. Sep. Sci. 31, 1449–1464 (2008).
D. V. McCalley, Study of selectivity, retention mechanism and performances of alternative silica based stationary phases for separation of ionised solutes in hydrophilic interaction chromatography, J. Chromatogr. A 1217, 3408–3417 (2010).
A. E. Karatapanis, Y. C. Fiamegos, C.D. Stalikas, Study of the behavior of water- soluble vitamins in HILIC on a diol column, Chromatographia 71, 751–759 (2010).
A. E. Karatapanis, Y. C. Fiamegos, C.D. Stalikas, A revise to the retention mechanism of hydrophilic interaction liquid chromatography using model organic compounds, J. Chromatogr.A 1218, (2011) 2871–2879.
A. C. Moffat, M. D. Osselton, B. Widdop Eds., Clarke’s Isolation and Identification of Drugs. The Pharmaceutical Society of Great Britain, London, England 1986.
Y. Guo, S. Gaiki, Retention behavior of small polar compounds on polar stationary phases in hydrophilic interaction chromatography, J. Chromatogr. A 1074, 71–80 (2005).
G. B. Cox, R. W. Stout, Study of the retention mechanism for basic compound on silica under pseudo-reversed conditions, J. Chromatogr. 384, 315–336 (1987).
X. Yang, J. Dai, P. W. Carr, Analysis and critical comparison of the reversed-phase and Ion-exchange contribution to retention on polybutadiene coated zirconia and octadecyl silane bonded silica phases, J. Chromatogr. A 996, 13–31(2003).
International Conference on Harmonization Techical Requirements for Registration of Pharmaceuticals for Human Use Guideline on Validation of Analytical Procedures: Text and Methodology Q2(R1), Geneva, Switzerland (2005).
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