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Development and Validation of an HPLC Method for Simultaneous Determination of Ibuprofen and 17 Related Compounds

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Abstract

A reversed-phase high-performance liquid chromatography (RP-HPLC) method was developed and validated for determination of ibuprofen and 17 related compounds (chemical process impurities and degradation products) simultaneously. This method may be used for quality control of ibuprofen-containing substances. A number of chromatographic parameters (column, flow rate, temperature, wavelength, gradient elution, buffer solution, and pH) were evaluated. An Agilent ZORBAX Eclipse Plus C18 (250 × 4.6 mm, 5 μm particle size) column at 40 °C was selected on the basis of its separation efficiency and robustness. The column was eluted at 1.0 mL min−1 with a gradient using 10 mM sodium phosphate buffer at pH 6.9 as mobile phase A and acetonitrile as mobile phase B. The ultraviolet detector was set at 214 nm. This method was validated to confirm its system suitability, specificity, linearity, precision, accuracy, sensitivity, robustness, and sample stability according to international conference on harmonization (ICH) guidelines. This method was applied to analyze seven batches of ibuprofen drug products from different manufacturers.

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References

  1. Jasani MK, Downie WW, Samuels BM, Buchanan WW (1968) Ibuprofen in rheumatoid arthritis. Clinical study of analgesic and anti-inflammatory activity. Ann Rheum Dis 27:457–462

    Article  CAS  Google Scholar 

  2. Brayfield A (2014) Martindale: the complete drug reference. Royal Pharmaceutical Society, London

    Google Scholar 

  3. Goodman LS, Gilman A (1990) Goodman and Gilman’s pharmacological basis of therapeutics, 8th edn. Pergamon, New York

    Google Scholar 

  4. Shioiri T, Kawai N (1978) New methods and reagents in organic synthesis. 2. A facile conversion of alkyl aryl ketones to α-arylalkanoic acids using diphenyl phosphorazidate. Its application to a new synthesis of ibuprofen and naproxen, nonsteroidal antiinflammatory agents. J Org Chem 43:2936–2938

    Article  CAS  Google Scholar 

  5. Ghosh S, Pardo SN, Salomon AG (1982) Ester enolates from α-acetoxy esters. Synthesis of arylmalonic and α-arylalkanoic esters from aryl nucleophiles and α-keto esters. J Org Chem 47:4692–4702

    Article  CAS  Google Scholar 

  6. Pinhey JT, Rowe BA (1980) The α-arylation of derivatives of malonic acid with aryllead triacetates. New syntheses of ibuprofen and phenobarbital. Tetrahedr Lett 21:965–968

    Article  CAS  Google Scholar 

  7. Dondoni A, Dallocco T, Fantin G, Medici A, Pedrini P, Rossetti V (1986) Studies on the actual and potential impurities in ibuprofen. Il Farmaco 41:237–244

    CAS  Google Scholar 

  8. Huidobro AL, Rupérez FJ, Barba C (2006) Tandem column for the simultaneous determination of arginine, ibuprofen and related impurities by liquid chromatography. J Chromatogr A 1119:238–245

    Article  CAS  Google Scholar 

  9. Caviglioli G, Posocco V, Parodi V, Cafaggi S, Alzati A, Bignardi G (2002) Identification of degradation products of Ibuprofen arising from oxidative and thermal treatments. J Pharm Biomed Anal 30:499–509

    Article  CAS  Google Scholar 

  10. Gasco-Lopez AI, Izquiredo-Hornilos R, Jimenez A (1999) LC method development for ibuprofen and validation in different pharmaceuticals. J Pharm Biomed Anal 21:143–149

    Article  CAS  Google Scholar 

  11. Kučera R, Žižkovský V, Sochor J, Klimeš J, Dohnal J (2005) Utilization of zirconia stationary phase as a tool in drug control. J Sep Sci 28:1307–1314

    Article  Google Scholar 

  12. The United States Pharmacopeial Convention (2016) The United States Pharmacopeia 39. The National Formulary 30. United Book, Baltimore

    Google Scholar 

  13. Directorate for the Quality of Medicines (2016) The European Pharmacopoeia, supplement 9.1, 9th edn. Council of Europe, Strasbourg

    Google Scholar 

  14. Health Ministry, Stationery Office (2016) The British Pharmacopoeia, London

  15. Maggio RM, Vignaduzzo SE, Kaufman TS (2013) Practical and regulatory considerations for stability-indicating methods for the assay of bulk drugs and drug formulations. TrAC Trend Anal Chem 49:57–70

    Article  CAS  Google Scholar 

  16. Bartos D, Görög S (2008) Recent advances in the impurity profiling of drugs. Curr Pharm Anal 4:215–230

    Article  CAS  Google Scholar 

  17. Rao DD, Sait SS, Mukkanti K (2011) Development and validation of an UPLC method for rapid determination of ibuprofen and diphenhydramine citrate in the presence of impurities in combined dosage form. J Chromatogr Sci 49:281–286

    Article  CAS  Google Scholar 

  18. Li J, Xu L, Shi ZG, Hu M (2015) A novel two-dimensional liquid chromatographic system for the online toxicity prediction of pharmaceuticals and related substances. J Hazard Mater 293:15–20

    Article  CAS  Google Scholar 

  19. Haikala VE, Heimonen IK, Vuorela HJ (1991) Determination of ibuprofen in ointments by reversed-phase liquid chromatography. J Pharm Sci 80:456–458

    Article  CAS  Google Scholar 

  20. Kalafut P, Kučera R, Klimeš J, Sochor J (2009) An innovative approach to the analysis of 3-[4-(2-methylpropyl)phenyl] propanoic acid as an impurity of ibuprofen on a carbon-coated zirconia stationary phase. J Pharm Biomed Anal 49:1150–1156

    Article  CAS  Google Scholar 

  21. Persson-Stubberud K, Astrom O (1998) Separation of ibuprofen, codeine phosphate, their degradation products and impurities by capillary electrophoresis—I. Method development and optimization with fractional factorial design. J Chromatogr A 798:307–314

    Article  CAS  Google Scholar 

  22. Kučera R, Sochor J, Klimeš J, Dohnal J (2005) Use of the zirconia-based stationary phase for separation of ibuprofen and its impurities. J Pharm Biomed Anal 38:609–618

    Article  Google Scholar 

  23. Quaglia MG, Donati E, Fanali S, Catarcini P (2003) Ibuprofen quality control by electrochromatography. Farmaco (Lausanne) 58:699–705

    Article  CAS  Google Scholar 

  24. Elzanfaly ES, Zaazaa HE, Soudi AT, Salem MY (2015) Development and validation of chromatographic methods for simultaneous determination of ibuprofen and famotidine in presence of related substances in pharmaceutical formulations. Acta Chim Slov 62:45–51

    CAS  Google Scholar 

  25. International Conference on Harmonization. ICH Q2(R1): Validation of analytical procedures-text and methodology, Geneva, Switzerland, 2005. http://www.ich.org. Accessed 7 Jun 2017

  26. Snyder LR, Kirkland JJ, Dolan JW (2010) Introduction to modern liquid chromatography, 3rd edn. Wiley, New York

    Google Scholar 

  27. Épshtein NA (2004) Validation of HPLC techniques for pharmaceutical analysis. Pharm Chem J 38:212–228

    Article  Google Scholar 

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Acknowledgements

This work was financially supported by the National Natural Science Foundation of China (No. 21322501, 21375005, 21275014).

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Authors and Affiliations

  1. College of Environmental and Energy Engineering, Bei**g University of Technology, Bei**g, People’s Republic of China

    Zunsheng Han, Li** Lu, Lin Wang & **ayan Wang

  2. Qilu Pharmaceutical (Hai Nan) Co., Ltd., Haikou, Hainan, People’s Republic of China

    Zimeng Yan

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  1. Zunsheng Han
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  2. Li** Lu
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  3. Lin Wang
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  4. Zimeng Yan
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Correspondence to Zimeng Yan or **ayan Wang.

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Han, Z., Lu, L., Wang, L. et al. Development and Validation of an HPLC Method for Simultaneous Determination of Ibuprofen and 17 Related Compounds. Chromatographia 80, 1353–1360 (2017). https://doi.org/10.1007/s10337-017-3358-3

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  • DOI: https://doi.org/10.1007/s10337-017-3358-3

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