RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND DEXAMETHASONE IN EYE/EAR DROPS
Abstract
High performance liquid chromatography method was applied to the simultaneous determination of ciprofloxacin and dexamethasone. The chromatographic separation was achieved on reversed-phase C18 column(25 cm × 4.6 mm id, 5 µm) in the isocratic mode using methanol-water-triethylamine (55:45:0.6, v/v/v), pH adjusted to 3.0 ± 0.05 with orthophosphoric acid as the mobile phase at a flow rate 0.8 ml/min. Quantitation was achieved with UV detection at 254 nm. In the HPLC method, quantification was achieved over the concentration range of 3-18 and 1-6µg/ml, with mean recoveries of 99.94 ± 1.51 and 100.28 ± 1.25% for ciprofloxacin and dexamethasone respectively. The proposed methods were successfully applied for the analysis of synthetic mixtures and pharmaceutical formulations of ciprofloxacin and dexamethasone without any interference from common excipients.
Keywords:
Ciprofloxacin, Dexamethasone, Liquid Chromatography, ValidationDOI
https://doi.org/10.25004/IJPSDR.2013.050205References
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29. Francesco RD, Frerichs V, Donnelly J, Hagler C, Hochreiter J, Tornatore KM. Simultaneous determination of cortisol, dexamethasone, methylprednisolone, prednisone, prednisolone, mycophenolic acid and mycophenolic acid glucuronide in human plasma utilizing liquid chromatography–tandem mass spectrometry. J. Chromatogr. B. 2007; 859:42-51.
30. Yang Y, Li H, Gao K, Liu M, Sun Y, Yan T, Fawcett JP, Cui Y, Gu J. Simultaneous quantitation of dexamethasone palmitate and dexamethasone in human plasma by liquid chromatography/tandem mass spectrometry. J. Chromatogr. B. 2008; 862:119-124.
31. Hidalgo OH, Lopez MJ, Carazo EA, Larrea MSA, Reuvers TBA. Determination of dexamethasone in urine by gas chromatography with negative chemical ionization mass spectrometry. J. Chromatogr. B. 2003; 788:137-146.
32. Spektor Z, Jasek MC, Jasheway D, Dahlin DC, Kay DJ, Mitchell R, Faulkner R, Wall GM. Pharmacokinetics of CIPRODEX® otic in pediatric and adolescent patients. Int. J. of Pediatr. Otorhinolaryngol. 2008; 72:97-102.
33. Conroy PJ. New Quinolone/Steroid combination for topical treatment of acute otitis: Early- and late-phase study results. ENT J. 2003; 82: 1-4.
34. Moe BR, Dupre S, Wall M, Stroman D, Celeste McLean Joseph Dohar, Giles W, Roland P. Bikhazi N, Carroll S, Crenshaw K. Topical Ciprofloxacin/Dexamethasone Superior to Oral Amoxicillin/Clavulanic Acid in Acute Otitis Media with Otorrhea through Tympanostomy Tubes. Pediatrics. 2006; 118:1-9.
35. Ermis SS, Aktepe OC, Inan UU, Ozturk F, Altindis M. Effect of topical dexamethasone and ciprofloxacin on bacterial flora of healthy conjunctiva. Eye. 2004; 18:249-252.
36. Synder LR, Kirkland JJ, Glajck JL. Practical HPLC Method Development, John Wiley & Sons, Inc.: New York, 1997.
37. ICH Topic Q2B, Note for Guidance on Validation of Analytical Procedures: Methodology GPMP/ICH/281/95, The European Agency for the Evaluation of Medical Products: Geneva, 1996.
2. Sweetman SC. Martindale, The complete Drug Reference, 36th Ed., Pharmaceutical Press: London, 2009.
3. Hardman JG, Limbird LE. Goodman and Gilman, The Pharmacologic Basis of Therapeutics, 11th Ed., McGraw-Hill: New York, 2006.
4. Kilic E, Koseoglu F, Akay MA. Non-aqueous titrimetric assay of selected antibiotics using tetra-N-butylammonium hydroxide as titrant. J. Pharm. Biomed. Anal. 1994; 12:347.
5. Patel SA, Patel NM, Patel MM. Simultaneous spectrophotometric estimation of ciprofloxacin and ornidazole in tablets. Indian J. Pharm. Sci. 2006; 68:665-667.
6. Amin AS. Spectrophotometric microdetermination of some important aminoquinoline antimalarials, as ion-pair complex. Mikrochim. Acta. 2000; 134:89-94.
7. Abdel-Gawad FM, Issa YM, Fahmy HM, Hussein HM. Spectrophotometric determination of ciprofloxacin in pure form and in tablets through charge-transfer complexation reactions. Mikrochim. Acta. 1998; 130:35.
8. Rizk M, Balal F, Ibrahim F, Ahmed S, Sheribah Z.A. Derivative Spectrophotometric Analysis of 4-Quinolone Antibacterials in Formulations and Spiked Biological Fluids by Their Cu (II) Complexes. J. AOAC Int. 2001; 84: 368.
9. Witte BD, Dewulf J, Demeestere K, Ruyck MD, Langenhove HV. Critical points in the analysis of ciprofloxacin by high-performance liquid chromatography. J. Chromatogr. A. 2007; 1140:126-130.
10. Belal F, Al-Majed,AA, Al-Obaid AM. Methods of analysis of 4-quinolone antibacterials. Talanta, 1999; 50:765-786.
11. Joshi S. HPLC separation of antibiotics present in formulated and unformulated samples. J. Pharm. Biomed. Anal. 2002; 28:795-809.
12. Shervington LA, Abba M, Hussain B, Donnelly J. Simultaneous separation and determination of five quinolone antibotics using isocratic reversed-phase HPLC: Application to stability studies on an ofloxacin tablet formulation. J. Pharm. Biomed. Anal. 2005; 39: 769-775.
13. Kassab NJ. Singh AK, Hackmam ERMK, Santoro MIRM. Quantitative determination of ciprofloxacin and norfloxacin in pharmaceutical preparations by high performance liquid chromatography. Brazilian J. Pharm. Sci. 2005; 41:507-513.
14. Thoppil SO, Amin PD. Stability indicating reversed-phase liquid chromatographic determination of ciprofloxacin as bulk drug and in pharmaceutical formulations. J. Pharm. Biomed. Anal. 2000; 22:699-703.
15. Gomez DG, Anunciacion Espinosa-Mansilla, Arsenio Munoz de la Pena, Canada FC. HPLC determination of ciprofloxacin, cloxacillin and ibuprofen drugs in human urine samples. J. Pharm. Sci. 2006; 29:1969-1976.
16. Torniainen K, Mattinen J, Askolin CP, Tammilehto S. Structure elucidation of a photodegradation product of ciprofloxacin. J. Pharm. Biomed. Anal. 1997; 15:887-894.
17. Wang PL, Feng YL, Chen LA. Simultaneous Determination of Trace norfloxacin, pefloxacin, and ciprofloxacin by TLC–Fluorescence Spectrodensitometry. Microchem. J. 1997; 56:229-235.
18. Novakovic J, Nesmerak K, Nova H, Filka K. An HPTLC method for the determination and the purity control of ciprofloxacin HCl in coated tablets. J. Pharm. Biomed. Anal. 2001; 25:957-964.
19. Michalska K, Pajchel G, Tyski S. Determination of ciprofloxacin and related impurities by capillary zone electrophoresis. J. Chromatogr. A. 2004; 1051:267-272.
20. Altria KD, Chanter YL. Validation of a capillary electrophoresis method for the determination of a quinolone antibiotic and its related impurities. J. Chromatogr. A. 1993; 652:459-463.
21. Michalska K, Pajchel G, Tyski S. Determination of ciprofloxacin and related impurities by capillary zone electrophoresis. J. Chromatogr. A. 2004; 1051:267-272.
22. Graham RE, Williams PA, Kenner CT. Detection of decomposition and analytical interferences in pharmaceutical preparations containing corticosteroids. J. Pharm. Sci. 1970; 59:1152-1156.
23. Pendela M, Adams E, Hoogmartens J. Development of a liquid chromatographic method for ear drops containing neomycin sulphate, polymyxin B sulphate and dexamethasone sodium phosphate. J. Pharm. Biomed. Anal. 2004; 36:751-757.
24. Xiong Y, Xioa KP, Rustum AM. Development and validation of a stability-indicating RP-HPLC method to separate low levels of dexamethasone and other related compounds from betamethasone. J. Pharm. Biomed. Anal. 2009; 49:646-654.
25. Volin P. HPLC analysis of corticosteroids. J. Chromatogr. B. 1995; 671:319-340.
26. United States Pharmacopoeia (30) National Formulary 25, The United States Pharmacopoeial Convention: Rockville, 2007.
27. Gagliardi L, Orsi DD, Giudice MRD, Gatta F, Porrà R, Chimenti P, Tonelli D. Development of tandem thin-layer chromatography-high-performance liquid chromatography method for the identification and determination of corticosteroids in cosmetic products. Anal. Chim. Acta. 2002; 457:187-198.
28. Wasch KD, Brabender HFD, Wiele MVD, Vercammen J, Courtheyn D, Impens S. Differentiation between dexamethasone and betamethasone in a mixture using multiple mass spectrometry. J. Chromatogr. A. 2001; 926:79-86.
29. Francesco RD, Frerichs V, Donnelly J, Hagler C, Hochreiter J, Tornatore KM. Simultaneous determination of cortisol, dexamethasone, methylprednisolone, prednisone, prednisolone, mycophenolic acid and mycophenolic acid glucuronide in human plasma utilizing liquid chromatography–tandem mass spectrometry. J. Chromatogr. B. 2007; 859:42-51.
30. Yang Y, Li H, Gao K, Liu M, Sun Y, Yan T, Fawcett JP, Cui Y, Gu J. Simultaneous quantitation of dexamethasone palmitate and dexamethasone in human plasma by liquid chromatography/tandem mass spectrometry. J. Chromatogr. B. 2008; 862:119-124.
31. Hidalgo OH, Lopez MJ, Carazo EA, Larrea MSA, Reuvers TBA. Determination of dexamethasone in urine by gas chromatography with negative chemical ionization mass spectrometry. J. Chromatogr. B. 2003; 788:137-146.
32. Spektor Z, Jasek MC, Jasheway D, Dahlin DC, Kay DJ, Mitchell R, Faulkner R, Wall GM. Pharmacokinetics of CIPRODEX® otic in pediatric and adolescent patients. Int. J. of Pediatr. Otorhinolaryngol. 2008; 72:97-102.
33. Conroy PJ. New Quinolone/Steroid combination for topical treatment of acute otitis: Early- and late-phase study results. ENT J. 2003; 82: 1-4.
34. Moe BR, Dupre S, Wall M, Stroman D, Celeste McLean Joseph Dohar, Giles W, Roland P. Bikhazi N, Carroll S, Crenshaw K. Topical Ciprofloxacin/Dexamethasone Superior to Oral Amoxicillin/Clavulanic Acid in Acute Otitis Media with Otorrhea through Tympanostomy Tubes. Pediatrics. 2006; 118:1-9.
35. Ermis SS, Aktepe OC, Inan UU, Ozturk F, Altindis M. Effect of topical dexamethasone and ciprofloxacin on bacterial flora of healthy conjunctiva. Eye. 2004; 18:249-252.
36. Synder LR, Kirkland JJ, Glajck JL. Practical HPLC Method Development, John Wiley & Sons, Inc.: New York, 1997.
37. ICH Topic Q2B, Note for Guidance on Validation of Analytical Procedures: Methodology GPMP/ICH/281/95, The European Agency for the Evaluation of Medical Products: Geneva, 1996.
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01-04-2013
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“RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND DEXAMETHASONE IN EYE EAR DROPS”. International Journal of Pharmaceutical Sciences and Drug Research, vol. 5, no. 2, Apr. 2013, pp. 62-66, https://doi.org/10.25004/IJPSDR.2013.050205.
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How to Cite
“RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF CIPROFLOXACIN AND DEXAMETHASONE IN EYE EAR DROPS”. International Journal of Pharmaceutical Sciences and Drug Research, vol. 5, no. 2, Apr. 2013, pp. 62-66, https://doi.org/10.25004/IJPSDR.2013.050205.
