http://dx.doi.org/10.5935/sc.2019.009

Clean, safe and fast method by HPLC for quantification of rifaximin-based samples

Kogawa A. C., Peltonen L., Salgado H. R. N., Chorilli M.

Keywords: rifaximin-based samples, HPLC, analytical method validation, quality control, pharmaceutical analysis.

Abstract: Rifaximin, is an oral antimicrobial drug, belongs to Class IV, according to the Biopharmaceutic Classification System, and has low solubility and permeability. Three rifaximin-based samples were developed by complexation to β-cyclodextrin using phase solubility diagram and malaxation, and decreasing particle size using wet milling. The effectiveness of preparation of new rifaximin-based samples has been previously confirmed and characterized by thermal and spectroscopic techniques, but the quantification of rifaximin has not yet been performed because there is no method available. So an ecologically correct method by HPLC was developed and validated to evaluate the rifaximin content in them. The analysis was performed using a C18 column, water with 0.1% glacial acetic acid and ethanol (52:48, v/v) as mobile phase, 0.9 mL min-1, 290 nm, and 25°C. The method proved to be linear in the range of 5-50 μg mL-1 and precise with relative standard deviations of 1.15% for intra-day and 0.47% for inter-day precision. Accuracy was confirmed by standard recovery with mean recoveries between 100.99 and 101.32%. The method was robust to small changes in wavelength and temperature used, purified water source, the proportion of ethanol and acetic acid in the mobile phase and flow. Selectivity was confirmed by the evaluation of possible interferences and forced degradation tests in acidic, basic, oxidative, neutral, and photolytic media and it proved to be indicative of stability. The method also involves characteristics of green Analytical Chemistry for a pharmaceutical analysis: it does not use toxic organic solvents, it is fast (approximately 5 minutes), and waste generation is low.


Referências Bibliográficas

  1. Kogawa, A.C.; Salgado, H.R.N. Status of rifaximin: a review of characteristics, uses and analytical methods. Crit Rev Anal Chem. 2018;48:1-8.
  2. Rivkin, A.; Gim, S. Rifaximin: New Therapeutic Indication and Future Directions. Clin Ther. 2011;33:812-827.
  3. Mantry, P.S.; Mehta, A.; Graydon, R. Efficacy and tolerability of rifaximin in combination with lactulose in end-stage liver disease patients with MELD greater than 20: a single center experience. Transplant Proc. 2014;46:3481-3486.
  4. Pistiki, A.; Galani, I.; Pyleris, E.; Barbatzas, C.; Pimentel, M.; Giamarellos-Bourboulis, E.J. In vitro activity of rifaximin against isolates from patients with small intestinal bacterial overgrowth. Int J Antimicrob Agents. 2014;43:236-241.
  5. Castro, R.; Domenichelli, V.; Lorenzo, F.P.L.; Prestipino, M.; Perrotta, M.L. Rifaximin treatment for acute recurrent diarrhea in children with genitourinary disorders. Curr Therap Res. 1998;59:746-752.
  6. Ruiz, J.; Mensa, L.; O´Callaghan, C.; Pons, M.J.; González, A.; Vila, J.; Gascón, J. In vitro antimicrobial activity of rifaximin against enteropathogens causing traveler’s diarrhea. Diagn Micr Infec Dis. 2007;59:473-475.
  7. Zhang, X.; Duan, J.; Li, K.; Zhou, L.; Zhai, S. Sensitive quantification of rifaximin in human plasma by liquid chromatography–tandem mass spectrometry. J Chromatogr B. 2007;850:348-355.
  8. Jiang, Z.; Ke, S.; Dupont, H.L. Rifaximin – induced alteration of virulence of diarrhoea producing Escherichia coli and Shigella sonnei. Int J Antimicrob Agents. 2010;35:278-281.
  9. Valentin, T.; Leitner, E.; Rohn, A.; Zollner-Schwetz, I.; Hoenigl, M.; Salzer, H.J.F.; Krause, R. Rifaximin intake leads to emergence of rifampin-resistant staphylococci. J Infect. 2011;62:34-38.
  10. Mullen, K.D.; Sanyal, A.J.; Bass, N.M.; Poordad, F.F.; Sheikh, M.Y.; Frederick, T.; Bortey, E.; Forbes, W.P. Rifaximin is safe and well tolerated for long-term maintenance of remission from overt hepatic encephalopathy. Clin Gastroenterol Hepato. 2014;12:1390-1397.
  11. Kogawa, A.C.; Peltonen, L.; Antonio, S.G.; Salgado, H.R.N. Submission of rifaximin to different techniques: characterization, solubility study and microbiological evaluation. AAPS Pharm Sci Tech. 2019;20:125.
  12. Correa, C.B.M.; Kogawa, A.C.; Chorilli, M.; Salgado, H.R.N. Eco-friendly and miniaturized analytical method for quantification of rifaximin in tablets. Drug Analytical Research 2019;3:23-29.
  13. Kogawa, A.C.; Salgado, H.R.N. Quantification of rifaximin in tablets by spectrophotometric method ecofriendly in ultraviolet region. Scientifica 2016; 2016:1-9.
  14. Brbaklic, V.; Kogawa, A.C.; Salgado, H.R.N. Quantification of rifaximin in tablets by an environmentally friendly visible spectrophotometric method. Current Pharmaceutical Analysis 2017;13:532-537.
  15. Kogawa, A.C.; Salgado, H.R.N. Spectrophotometry in infrared region: a new, low cost and green way to analyze tablets of rifaximin. Current Pharmaceutical Analysis 2018;14:108-111.
  16. Kogawa, A.C.; Schepdael, A.V.; Salgado, H.R.N. Eco-friendly evaluation of rifaximin in tablets by capillary electrophoresis. Journal of Chromatographic Science 2019;57:476-483.
  17. Kogawa, A.C.; Mendonça, J.N.; Lopes, N.P.; Salgado, H.R.N. Method indicative of stability for the determination of rifaximin and its degradation products by thin chromatographic. Current Pharmaceutical Analysis 2017;13:520-524.
  18. Patel, K.G.; Jain, N.R.; Shah, P.A. Stability indicating HPTLC method for analysis of rifaximin in pharmaceutical formulations and an application to acidic degradation kinetic study. ISRN Analytical Chemistry 2013;613218:1-9.
  19. Sudha, T.; Hemalatha, P.V.; Ravikumar, V.R.; Jothi, R.; Radhakrishnan, M. Development and validation of RP-HPLC method for the estimation of rifaximin in bulk and in tablet dosage form. Asian Journal of Pharmaceutical and Clinical Research 2009;2:112-116.
  20. Kasimala, B.B.; Syed, R.; Pammi, K.; Sandhya, B. RP-HPLC method development and validation for the analyisis of rifaximin in pharmaceutical dosage forms. International Journal of Research and Reviews in Pharmacy and Applied Sciences 2011;1:323-333.
  21. Yong-jun, S.; Yun-gen, Y.. RP-HPLC determination related compounds of rifaximin. Anhui Chemical Industry 2008;1.
  22. International Conference on Harmonization. Validation of Analytical Procedures: Text and Methodology Q2(R1) 2005.
  23. Instituto Nacional de Metrologia, Normalização e Qualidade Industrial. Orientação sobre validação de métodos de ensaios químicos, DOQ-CGCRE-008 2007.
  24. Association of Official Analytical Chemists. Official Methods of Analysis. 20th ed, Rockville: AOAC International 2016.
  25. Agência Nacional de Vigilância Sanitária. Dispõe sobre a validação de métodos analíticos e dá outras providências. RDC n° 166, Brazil: ANVISA 2017.
  26. Kogawa, A.C.; Salgado, H.R.N. Impurities and forced degradation studies: a review. Curr Pharm Anal. 2016;12:18-24.
  27. Youden, W.J.; Steiner, E.H. Statistical manual of the AOAC. Association of Official Analytical Chemistry, Washington: DC, 1975.
  28. Association of Official Analytical Chemists. Guidelines for Single Laboratory Validation of Chemical Methods for Dietary Supplements and Botanicals, 2002.
  29. Horwitz, W.; Kamps, L.R.; Boyer, K.W.J. Quality assurance in the analysis of foods for trace constituents. Assoc Offic Anal Chem. 1980;63:1344-1355.
  30. World Health Organization 1993, http://www.inchem.org/documents/ehc/ehc/ehc154.htm, (access August 2019).
  31. World Health Organization 1997, http://www.inchem.org/documents/ehc/ehc/ehc196.htm (access August 2019).
  32. Kogawa, A.C.; Salgado, H.R.N. Ethanol on HPLC: Epiphany or Nonsense? Acta Sci Pharm Sci. 2018;2:14-15.
  33. Marco, B.A.; Rechelo, B.S.; Totoli, E.G.; Kogawa, A.C.; Salgado, H.R.N. Evolution of green chemistry and its multidimensional impacts: A review; Saudi Pharm J. 2019;27:1-8.