Cover Image

Development and Validation of an HPLC Method for the Determination of the macrolide antibiotic Clarithromycin using Evaporative Light Scattering Detector in raw materials and Pharmaceutical Formulations

Zampia Tzouganaki, Michael Koupparis

Abstract


In this work, ELS-Detector has been used for the development of an HPLC method for the determination of clarithromycin in pharmaceutical formulations (tablets and pediatric suspension). Isocratic reversed phase HPLC approach has been developed using a C-18 column (Waters Spherisorb 5 μm ODS2, 4.6x250 mm) and a mobile phase consisting of acetonitrile / aqueous trifluoroacetic acid as pairing reagent. Experimental parameters (temperature of heated drift tube, flow rate of mobile phase, gas flow rate, mobile phase composition) were optimized. Clarithromycin’ s stability was thoroughly examined in different solvent systems. Using the optimized conditions the working range was 5-100 μg/mL (upper limit can be increased considerably), with a detection limit of 4.5 μg/mL (6x10-6 M). The method was validated as per ICH guidelines. The retention time was 4.7 min. The method was successfully applied for the content assay of clarithromycin formulations.


Full Text:

PDF

References


- C.S. Young, J.W. Dolan, Success with Evaporative Light-Scattering Detection. LCGC North America, 2003, 21(2), 120-128.

- C.S. Young, J.W. Dolan, Success with Evaporative Light-Scattering Detection. Part II: Tips and Techniques, LCGC North America, 2004, 22(3), 244-250.

- B.H. Hsu, E. Orton, S.Y. Tang, R.A. Carlton, Application of evaporative light scattering detection to the characterization of combinatorial and parallel synthesis libraries for pharmaceutical drug discovery, J. Chromatogr. B, 1999, 725 (1), 103-112.

- H.J. Kim, I.K. Bae, M. H. Jeong, H.J. Park, J.S. Jung, J.E. Kim, A New HPLC-ELSD Method for Simultaneous Determination of

N-Acetylglucosamine and N-Acetylgalactosamine in Dairy Foods, Int. J. Anal. Chem., 2015, 892486.

- S. Han, K.Karlowicz-Bodalska, D. Szura, L. Ozimek, W. Musial, Application of HPLC with ELSD Detection for the Assessment of Azelaic Acid Impurities in Liposomal Formulation, Scientific World Journal, 2013, doi: 10.1155/2013/564962,URL: www.ncbi.nlm.nih.gov/pmc/articles /PMC3817643/.

- D. Montesano, L. Cossignani, L. Giua, E. Urbani, M. S. Simonetti, F. Blasi, A Simple HPLC-ELSD Method for Sugar Analysis in Goji Berry (Article ID 6271808), J. Chem, 2016, URLdoi.org/10.1155/2016/6271808.

- A. Pappa-Louisi, A. Papageorgiou, A. Zitrou, S. Sotiropoulos, E. Georgakis, F. Zougrou, Study on the electrochemical detection of the macrolide antibiotics clarithromycin and roxithromycin in reversed-phase high-performance liquid chromatography, J. Chromatogr. B, 2001, 755 (1-2), 57-64.

- I. Knafer, M.F.Skinner, R.B. Walker, Analysis of macrolide antibiotics. J. Chromatogr. A, 1998, 812(1), 255-286.

- P.O. Erah, D.A. Barret, P.N. Shaw, Ion-pair high-performance liquid chromatographic assay method for the assessment of clarithromycin stability in aqueous solution and in gastric juice, J. Chromatogr. B, 1982, 682 (1),73-78.

- S.J. Choi, S.B. Kim, H.Y. Lee, D.H. Na, Y.S. Yoon, S.S. Lee, J.H. Kim, K.C. Lee, H.S. Lee, Column-Switcing High Performance Liquid Chromatographic determination of clarithromycin in human plasma with electorchemical detection. Talanta, 2001, 54 (2), 377-382.

- J. Sastre-Torano, H.J. Guchelaar, Quantitative determination of the macrolide antibiotics erythromycin, roxithromycin, azithromycin and clarithromycin in human serum by high-performance liquid chromatography using pre-column derivatization with 9-fluorenylmethyloxycarbonyl chloride and fluorescence detection J. Chromatogr. B, 1998, 720 (1-2),89-97.

- F.S. Kees, M. Spangler, M.Wellenhofer, Determination of macrolides in biological matrices by high-performance liquid chromatography with electrochemical detection, J. Chromatogr. A, 1998, 812 (1-2), 287-292.

- S.Y. Chu, L.T. Sennello, R.C. Sonders, Simultaneous determination of clarithromycin and 14(R)-hydroxyclarithromycin in plasma and urine using high-performance liquid chromatography with electrochemical detection, J. Chromatogr. A, 1991, 571 (1-2), 199-208.

- M. Hendenmo, B.M. Eriksson, Liquid chromatographic determination of the macrolide antibiotics roxithromycin and clarithromycin in plasma by automated solid phase extraction and electrochemical detection, J. Chromatogr. A, 1995, 692(1-2),161-166.

- W. Li, H. Jia, K. Zhao, Determination of clarithromycin in rat plasma by HPLC-UV method with pre-column derivatization, Talanta, 2007, 71(1), 385-390.

- P.Y. Khasaba, Spectrofluorimetric analysis of certain macrolide antibiotics in bulk and pharmaceutical formulations. J. Pharm. Biomed. Analysis, 2002, 27 (6), 923-932.

- J. Shah, R. Jan, R. Manzour, Extractive Spectrophotometric methods for the determination of clarithromycin in pharmaceutical formulations using bromothymol blue and cresol red, J. Chin. Chem. Soc, 2008, 55(5),1107-1112.

- F. Sacher, F.T. Lange, H.J. Brauch, I. Blankenhorn, Pharmaceuticals in groundwaters: Analytical methods and results of a monitoring program in Baden-Württemberg, Germany, J. Chromatogr. A, 2001, 938(1-2),199-210.

- S. Oswald, J. Peters, M. Venner, W. Siegmund, LC-MS/MS method for the simultaneous determination of clarithromycin, rifampicin and their main metabolites in horse plasma, epithelial lining fluid and broncho- alveolar cells, J. Pharm. Biomed. Analysis, 2011, 55(1), 194-201.

- S.H. Zhang, X.A. Huang, N.S. Yao, C. Horvath, Preparation of monodisperse porous polymethacrylate microspheres and their application in the capillary electrochromatography of macrolide antibiotics, J. Chromatogr. A, 2002, 948 (1-2), 193-201.

- K.O.Abuga, H.K.Chepkwony, E. Roets, J. Hoogmartens, A stability-indicating HPLC method for the separation of clarithromycin and related substances in bulk samples, J. Sep. Sci. 2001, 24(10-11), 849-855.

- C. Taninaka, H. Ohtani, E. Hanada, H. Kotaki, H. Sato, T. Iga, Determination of erythromycin, clarithromycin, roxithromycin, and azithromycin in plasma by high-performance liquid chromatography with amperometric detection, J. Chromatogr. B, 2000, 738 (2),405-411.

- C.L. Flurer, Analysis of macrolide antibiotics by capillary electrophoresis, Electrophoresis 1996, 17(2), 359-366.

- L. Qingying, L. Jiufeng, S.Xuqin, Z. Meiyu, L. Erfen, G. Fuming, H. Limin, Simultaneous determination of aminoglycoside antibiotics in feeds using high-performance liquid chromatography with evaporative light scattering detection, RSC Adv., 2017, 7, 1251-1259, DOI: 10.1039/C6RA26581B.

- B.J. Yaan, S.Z. Tai, HPLC-ELSD determination of content of clarithromycin capsules, Ch. Pract. Med., 2009,25.

- A. Bharathi, Y.H. Wang, T. Smillie, W. Mabusel, L. Vincent, F. Weitz, I. Khan,

- Comparison of LC-UV, LC-ELSD, and LC-MS methods for the determination of sesquiterpenoids in various species of Artemisia, Chormatographia, 2006, 70 (5), 797- 803.

- N. Megoulas, M.A. Koupparis, Development and validation of a novel LC/ELSD method for the quantitation of gentamicin sulfate components in pharmaceuticals, J. Pharm. Biomed. Anal. , 2004,36(1),73-79.

- V. Douville , A. Lodi, J. Miller, A. Nicolas, I. Clarot, B. Prilleux , N. Megoulas , M. Koupparis M, Pharmeur. Sci. Notes, 2006, (1),9-15.

- S.N. Alvi, S. A. Dgither, M. M Hammami, Rapid Determination of Clarithromycin in Human Plasma by LCMS/MS Assay, Pharm. Anal. Chem, 2016, 2(1),110. url: dx.doi.org/10.4172/2471-2698.1000110.

- P. Grübel , D.R. Cave , Factors affecting solubility and penetration of clarithromycin through gastric mucus Aliment, Pharmacol. Ther., 1998, 2(6),569-576.

- I.I. Salem, Clarithromycin, Anal Profiles Drug Subst Excipients, 1996, 24 (II-XI), 45-85.

- European Pharmacopeia (Eu. Ph. 9th), 2.2.46 Chromatographic Separation Techniques, 9.2-4286.

- Stability Testing of New Active Substances and Medicinal Products, ICH Topic Q1A, ICH Harmonized Tripartite Guidelines, ICH, Surrey, U.K.,1996, CPMP/ICH/280/95.

- United States Pharmacopeia, National Formulary, Validation of Compendial Methods Rockville, MD, 2011, 1225, 549.




DOI: http://dx.doi.org/10.13171/mjc64/01706211420-tzouganaki

Refbacks

  • There are currently no refbacks.


Copyright (c) 2017 Mediterranean Journal of Chemistry