DEVELOPMENT AND VALIDATION OF A HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF PSEUDOEPHEDRINE, DEXTROMETHORPHAN, AND TRIPROLIDINE IN THEIR COMBINED COUGH AND COLD SYRUPS
DOI:
https://doi.org/10.24297/jac.v13i11.5911Keywords:
cation exchange column, pseudoephedrine, dextromethorphan, triprolidine, experimental designAbstract
A simple and efficient liquid chromatographic method has been developed and validated for the simultaneous determination of pseudoephedrine, dextromethorphan, and triprolidine in cough and cold syrup. The separation of the analytes was achieved within 10min, employing a mixture of 50% v/v methanol-water containing 35.07 mM/L ammonium acetate adjusted to pH 5.58 as isocratic mobile phase, pumped at 1.0 ml min-1 through a strong cation exchange column (10µm particle size). The analytes were detected at 265nm. Statistical experimental designs and graphic representations (response surface methodologies, Pareto charts) were used for optimizing the mobile phase composition. The linearity of the calibration (r>0.99, n =18) in the relevant ranges (up to 125% of the expected concentrations of the analytes in the formulation), method accuracy (RSD <2.0%), repeatability (RSD<2.0%) and intermediate precision, were verified. System suitability parameters were also determined. The validated method was successfully employed for the routine analysis of a syrup pharmaceutical preparation against cough and cold, showing satisfactory analytes recoveries and precsion.
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References
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[27] S. Di Berardino, R. Jasionowska, Rapid and Sensitive CZE Method for Quality Control Analysis of Pharmaceuticals Containing Pseudoephedrine, Triprolidine and Paracetamol. American J. Anal. Chem. 5, 613-619 (2014).
[28] L. Zhang, Q. Hu, G. Chen, Y. Fang, Simultaneous determination of the active ingredients in composite pseudoephedrine hydrochloride tablets by capillary electrophoresis. Anal. Chim.Acta. 424, 257–262 (2000).
[29] J.L. Murtha, T.N. Julian, GW Radebau, Simultaneous Determination of Pseudoephedrine Hydrochloride, Chlorpheniramine Maleate, and Dextromethorphan Hydrobromide by Second-Derivative Photodiode Array Spectroscopy. J. Pharm. Sci. 47,715-718 (1988)
[30] A.G. Davidson, L.M.M. Mkoji, The simultaneous assay of triprolidine, pseudoephedrine and dextromethorphan in combined preparations by derivative-difference spectrophotometry . J. Pharm. Biomed. Anal. 6, 449-460 (1988).
[31] Ö.A. Dönmez, A. Bozdoğan, G. Kunt, Determination of Ternary Mixtures of Dextromethorphan Hydrobromide, Pseudoephedrine Hydrochloride and Triprolidine Hydrochloride in Syrups by Partial Least-Squares Multivariate Calibration. Reviews in Anal. Chem. 26(3), 209-217 (2007).
[32] R. Jones, M.I. Orchard, K. Hall, The use of derivative and least-squares methods to analyse a polypharmaceutical product by UV spectrophotometry. J. Pharm. Biomed. Anal. 3, 335-342 (1985).
[33] D. De Orsi, L. Gagliardi, A. Bolasco, D. Tonelli, Simultaneous determination of triprolidine, pseudoephedrine, paracetamol and dextromethorphan by HPLC. Chromatographia. 43, 496-500 (1996).
[34] S. Furlanetto, S. Orlandini, How Experimental Design Can Improve the Validation Process. Studies in Pharmaceutical Analysis. Anal. Bioanal. Chem. 377, 937–944 (2003).
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[36] H.T. Ting, K.A. Abou El-Hossein , H.B. Chua, J. Scientific & Industrial Research. 6, 11 (2009).
[37] G.E.P. Box, D.W. Behnken Some new three-level designs for the study of quantitative variables. Technometrics. 2, 455-475 (1960).
[38] G. Derringer, R. Suich. Simultaneous Optimization of Several Response Variables. J. Qual. Technol. 12, 214-219 (1980).
[39] A.C. Moffat, M.D. Osselton, B. Widdop, Clarke’s Analysis of Drugs and Poisons, 4th Ed., , London, England, UK: Pharmaceutical Press. (2011).
[40] K. Cores, P.T. McCarthy, R.J. Flanagan, HPLC of basic drugs and quaternary ammonium compounds on microparticulate strong cation-exchange materials using methanolic or aqueous methanol eluents containing an ionic modifier. J Chromatogr A. 693, 289-306 (1995).
[41] J. Ermer, E.R. Miller, Method Validation in Pharmaceutical Analysis - A Guide to Best Practice. Weinheim:Wiley-VCH Verlag GmbH & Co, KGaA (2005).
[42] J.R. Jenke Chromatographic method validation: A review of current practices and procedures. Part III. Ruggedness, revalidation and system suitability. J. Liq. Chromatogr. 19(12), 1873–1891 (1996).
[2] N. Borkar, S. Sawant, Review of Simultaneous Determination of Analytes by High Performance Liquid Chromatography (HLPC) in Multicomponent Cough and Cold Oral Drug Products. Int. J. Pharm. Tech. Res. 3, 1339-1345 (2011).
[3] S. Sweetman, Martindale: The Complete Drug Reference, The Pharmaceutical Press. (London, 2009).
[4] B.Law, JRG. Appleby, Re-evaluation of strong cation-exchange high-performance liquid chromatography for the analysis of basic drugs. J. Chromatogr. A. 725, 335-341 (1996)
[5] R.J. Flanagan , E.J. Harvey, E.P. Spencer, HPLC of basic drugs on microparticulate strong cation-exchange materials - a review. Fore. Sci. Int. 121, 97-102 (2001).
[6] Z. Long, C. Wang, Z. Guo, X. Zhang, L. Nordahl, X. Liang, Strong cation exchange column allow for symmetrical peak shape and increased sample loading in the separation of basic compounds. J. Chromatogr. A. 1256, 67-71 (2012).
[7] L. Sriphong, A. Chaidedgumjorn, K. Chaisuroj, Derivative Spectrophotometry Applied to the Determination of Triprolidine Hydrochloride and Pseudoephedrine Hydrochloride in Tablets and Dissolution Testing.World Academy of Science, Engineering and Technology. 55, 573-577 (2009).
[8] R. Moharana, N. Kawathekar, S.C. Chaturvedi, Simultaneous Spectrophotometric Estimation Of Triprolidine Hydrochloride And Pseudoephedrine Hydrochloride In Pharmaceutical Dosage Form. Indian J Pharm. Sci . 58, 93-95 (1996).
[9] M.J. Akhtar, S. Khan, M. Hafiz, High-performance liquid chromatographic assay for the determination of paracetamol, pseudoephedrine hydrochloride and triprolidine hydrochloride. J. Pharm. Biomed. Anal. 12, 379-382 (1994).
[10] D.B. Wanjari , V.V. Parashar, S.N. Lulay, M.R. Tajne, N.J. Gaikwad, Simultaneous HPLC estimation of acetaminophen, chlopheniramine maleate, dextromethorphan hydrobromide and pseudoephedrine hydrochloride in tablets. Indian J. of Pharm. Sci. 66, 345-347 (2004).
[11] K.C. Marcus, J.H. Ira, A.F. Salvatore, Ion-Pair Reversed-Phase High-pressure Liquid Chromatography of Cough-Cold Syrups I: Pseudoephedrine Hydrochloride, Brompheniramine Maleate, and Dextromethorphan Hydrobromide. J. Pharm. Sci. 68,1463-1464 (1979).
[12] F. Al-Rimawi, Normal-phase LC method for simultaneous analysis of pseudophedrine hydrochloride, dextromethorphan hydrobromide, chlorpheniramine maleate, and paracetamol in tablet formulations. Saudi Pharm. J. 18, 103–106 (2010).
[13] M. Qi, P. Wang, L. Zhou, Y. Sun, Simultaneous Determination of Four Active Components in a Compound Formulation by Liquid Chromatography. Chromatographia. 58, 183-186 (2003).
[14] A. Manassra, M. Khamis, M. El-Dakiky, Z. Abdel-Qader, F. Al-Rimawi, Simultaneous HPLC analysis of pseudophedrine hydrochloride, codeine phosphate, and triprolidine hydrochloride in liquid dosage forms. J Pharm. and Biomed. Anal. 51, 991–993 (2010).
[15] M.S. Ali, M. Ghori, S. Rafiuddin, A.R. Khatri, A new hydrophilic interaction liquid chromatographic (HILIC) procedure for the simultaneous determination of pseudoephedrine hydrochloride (PSH), diphenhydramine hydrochloride (DPH) and dextromethorphan hydrobromide (DXH) in cough-cold formulations. J Pharm. Biomed. Anal. 43,158–167 (2007).
[16] C. Lei, N. Nan, Determination of Four Main Ingredients in Photifed -M Children Cough Syrup. Chinese J of Pharm. Anal. 24,44-45 (2004).
[17] B. Aşçı, O.A. Dönmez, A. Bozdoğan , S. Sungur, Simultaneous determination of paracetamol, pseudoephedrine hydrochloride, and dextromethorphan hydrobromide in tablets using multivariate calibration methods coupled with HPLC-DAD. J. Liq. Chromatog. Related Tech. 4, 1686-1698 (2011).
[18] H. Al-akraa, N. Sarkis, M Alshehaby, New rapid RP-HPLC method for simultaneous determination of some decongestants and cough-sedatives. Intern. J. Pharm. Pharm. Sci. 5, 234-241 (2013).
[19] M.R. Louhaichi, S. Jebali , M.H. Loueslati , N. Adhoum , L. Monser, Simultaneous determination of pseudoephdrine, pheniramine, guaifenisin, pyrilamine, chlorpheniramine and dextromethorphan in cough and cold medicines by high performance liquid chromatography. Talanta. 78, 991-997 (2009).
[20] U.R. Mallu, V. Bobbarala, S. Penumajji, Analysis of cough and analgesic range of pharmaceutical active ingredients using RP-HPLC. Intern. J. Pharma and Bio Sci. 2, 439-452 (2011).
[21] Y. El-Shabrawy, A. El-Gindy, M.A. Shoeib, Y. El-Gindy, An HPLC Method for Determination of 15 Pharmaceutical Compounds in Anti-Cold Products. Standard Research J. Pharm. Pharmacol. 1, 86-94 (2014).
[22] M.D. Pacioll, S.A. Jansen, S.A. Martellucci, A.A. Osei, A fast and efficient determination of amines and preservatives in cough and cold liquid and suspension formulations using a single isocratic ion-pairing high power liquid chromatography method . J. Pharm. Biomed. Anal. 26,143–149 (2001).
[23] R.K. Venisetty, S.K. Kumar, RP-HPLC Method Development and Validation for Simultaneous Estimation of Dextromethorphan , Phenylephrine and Triprolidine in Bulk and its Application in Evaluation of Marketed Tablet Dosage Forms. Int J of Adv. Biomed & Pharm Res. 3, 14-18 (2014).
[24] T. Harsono , M. Yuwono, G. Indrayar, Simultaneous determination of some active ingredients in cough-cold preparations by gas chromatography. JAOAC Int. 88, 1093-1098 (2005)
[25] O. Lau, Y. Cheung, Simultaneous determination of some active ingredients in cough-cold syrups by gas-liquid chromatography. Analyst. 115, 1349-1353 (1990)
[26] Y. Dong, X. Chen, Y. Chen , X. Chen, Z. Hu, Separation and determination of pseudoephedrine, dextromethorphan, diphenhydramine and chlorpheniramine in cold medicines by nonaqueous capillary electrophoresis. J. Pharm. Biomed. Anal. 39, 285–289 (2005).
[27] S. Di Berardino, R. Jasionowska, Rapid and Sensitive CZE Method for Quality Control Analysis of Pharmaceuticals Containing Pseudoephedrine, Triprolidine and Paracetamol. American J. Anal. Chem. 5, 613-619 (2014).
[28] L. Zhang, Q. Hu, G. Chen, Y. Fang, Simultaneous determination of the active ingredients in composite pseudoephedrine hydrochloride tablets by capillary electrophoresis. Anal. Chim.Acta. 424, 257–262 (2000).
[29] J.L. Murtha, T.N. Julian, GW Radebau, Simultaneous Determination of Pseudoephedrine Hydrochloride, Chlorpheniramine Maleate, and Dextromethorphan Hydrobromide by Second-Derivative Photodiode Array Spectroscopy. J. Pharm. Sci. 47,715-718 (1988)
[30] A.G. Davidson, L.M.M. Mkoji, The simultaneous assay of triprolidine, pseudoephedrine and dextromethorphan in combined preparations by derivative-difference spectrophotometry . J. Pharm. Biomed. Anal. 6, 449-460 (1988).
[31] Ö.A. Dönmez, A. Bozdoğan, G. Kunt, Determination of Ternary Mixtures of Dextromethorphan Hydrobromide, Pseudoephedrine Hydrochloride and Triprolidine Hydrochloride in Syrups by Partial Least-Squares Multivariate Calibration. Reviews in Anal. Chem. 26(3), 209-217 (2007).
[32] R. Jones, M.I. Orchard, K. Hall, The use of derivative and least-squares methods to analyse a polypharmaceutical product by UV spectrophotometry. J. Pharm. Biomed. Anal. 3, 335-342 (1985).
[33] D. De Orsi, L. Gagliardi, A. Bolasco, D. Tonelli, Simultaneous determination of triprolidine, pseudoephedrine, paracetamol and dextromethorphan by HPLC. Chromatographia. 43, 496-500 (1996).
[34] S. Furlanetto, S. Orlandini, How Experimental Design Can Improve the Validation Process. Studies in Pharmaceutical Analysis. Anal. Bioanal. Chem. 377, 937–944 (2003).
[35] ICH Guide Q2 (R1). Validation of Analytical Procedures - Text and Methodology. International Conference on Harmonization of Technical Requirements for Registration of Pharmaceuticals for Human Use (ICH), Geneva, Switzerland, (2005).
[36] H.T. Ting, K.A. Abou El-Hossein , H.B. Chua, J. Scientific & Industrial Research. 6, 11 (2009).
[37] G.E.P. Box, D.W. Behnken Some new three-level designs for the study of quantitative variables. Technometrics. 2, 455-475 (1960).
[38] G. Derringer, R. Suich. Simultaneous Optimization of Several Response Variables. J. Qual. Technol. 12, 214-219 (1980).
[39] A.C. Moffat, M.D. Osselton, B. Widdop, Clarke’s Analysis of Drugs and Poisons, 4th Ed., , London, England, UK: Pharmaceutical Press. (2011).
[40] K. Cores, P.T. McCarthy, R.J. Flanagan, HPLC of basic drugs and quaternary ammonium compounds on microparticulate strong cation-exchange materials using methanolic or aqueous methanol eluents containing an ionic modifier. J Chromatogr A. 693, 289-306 (1995).
[41] J. Ermer, E.R. Miller, Method Validation in Pharmaceutical Analysis - A Guide to Best Practice. Weinheim:Wiley-VCH Verlag GmbH & Co, KGaA (2005).
[42] J.R. Jenke Chromatographic method validation: A review of current practices and procedures. Part III. Ruggedness, revalidation and system suitability. J. Liq. Chromatogr. 19(12), 1873–1891 (1996).
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Published
2017-03-22
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Abu Reid, I. O., & Gad Kariem, E. A. (2017). DEVELOPMENT AND VALIDATION OF A HPLC METHOD FOR THE SIMULTANEOUS DETERMINATION OF PSEUDOEPHEDRINE, DEXTROMETHORPHAN, AND TRIPROLIDINE IN THEIR COMBINED COUGH AND COLD SYRUPS. JOURNAL OF ADVANCES IN CHEMISTRY, 13(11), 6011–6017. https://doi.org/10.24297/jac.v13i11.5911
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