Validated Spectrofluorimetric Determination of Gemifloxacin in Pharmaceutical Preparations and Spiked Human Plasma
DOI:
https://doi.org/10.24297/jac.v12i21.113Keywords:
Gemifloxacin mesylate, Spectrofluorimetry, AlCl3, SDS, Complexation, Pharmaceutical preparations and Biological Fluids.Abstract
 A simple, sensitive and rapid spectrofluorimetric method was developed and validated for the determination of Gemifloxacin mesylate (GFX), in bulk powder, pharmaceutical preparations and biological fluids. The proposed method was based on complexation of GFX with AlCl3 as complexing agent then measuring the fluorescence of the resulted complex after enhancement with sodium dodecyl sulphate (SDS) in borate buffer (pH 8) at emission wavelength of 401 nm after excitation at 264 nm. Different experimental parameters affecting the fluorescence intensity were carefully studied and optimized to obtain the maximum fluorescence intensity. The developed method was validated according to International Conference on Harmonisation guidelines in terms of specificity, linearity, lower limit of quantification (LOQ) 0.54 ng.ml-1, lower limit of detection (LOD) 0.18 ng.ml-1, accuracy and precision. The proposed method was found to be rectilinear over the concentration range of 1-20 ng.ml-1with recovery percentage of 99.85±0.84. The proposed method was applied successfully for the determination of GFX in pharmaceutical preparations and spiked human plasma with recovery percentage of 99.97±0.79 and 99.96±1.73 respectively. The results were statistically analyzed and compared with a reference method and no significance difference was found between both methods.
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References
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2. DomagaIa JM, Structure-activity and structure-side-effect reIationships for the quinoIone AntibacteriaIs. J Antimicrob Chemother 1994; 33: 685-706.
3. Ambadas, Rote R and PingIe SP, VaIidated UV-spectrophotometric methods for determination of gemifIoxacin mesyIate in pharmaceuticaI tabIet dosage forms. E J Chem, 7, 2010, 344-348.
4. AbdeI Wahed MG, EI Sheikh R, Gouda AA, and Abou TaIeb S, Kinetic spectrophotometric determination of gemifIoxacin mesyIate and moxifIoxacin hydrochIoride in pharmaceuticaI preparations using 4-ChIoro-7-nitrobenzo-2-oxa-1, 3-diazoIe. J Spectro, 2014, 2014, 1-12.
5. Hajera K and Zaheer Z, DeveIopment and VaIidation of a dissoIution test with spectrophotometric anaIysis for gemifIoxacin mesyIate and ambroxoI hydrochIoride in tabIet dosage form. J Pharm Tech Res, 4, 2012, 661-668.
6. Madhuri D, KottapaIIi CB, Devanna N and Somasekhar G. Direct and derivative spectrophotometric estimation of GemifIoxacin MesyIate by CheIation with Cr(III) Ion. Rasayan J.Chem, 3, 2010, 9-15.
7. Madhuri D, KottapaIIi CB, Devanna N and Somasekhar G, Direct and derivative spectrophotometric estimation of GemifIoxacin by cheIation with PaIIadium (II) Ion. Rasayan J.Chem, 3, 2010, 159-165.
8. EI-Bagary RI, Abo-taIib NF and N. EIdin MB, VaIidated StabiIity Indicating Assay of gemifIoxacin by different chromatographic and spectrophotometric methods of anaIysis. J. Chem Pharm Res, 3, 2011, 562-570.
9. Atia NN, Mahmoud AM, EI-Shabouri SR and EI-Koussi WM, Two vaIidated spectrofIuorometric methods for determination of gemifIoxacin mesyIate in tabIets and human pIasma. Int J AnaI Chem, 2013, 2013, 1-11.
10. Kepekci TSE and ÖnaI A, SpectrofIuorimetric methods for the determination of gemifIoxacin in tabIets and spiked pIasma sampIes. J FIuoresc., 21, 2011, 1001-7.
11. Moussa BA, Mahrouse MA, Hassan MA and Fawzy MG, SpectrofIuorimetric determination of gemifIoxacin mesyIate and IinezoIid in pharmaceuticaI formuIations. Acta Pharm, 64, 2014, 15-28.
12. AI-Tamimi SA, AIarfaj NA, AIy FA and AI-Mohaimeed AM, SpectrofIuorimetric anaIysis of gemifIoxacin mesyIate in pharmaceuticaI formuIations. Iumin, 29, 2014, 127-31.
13. EIbashir AA, Professor Saad B, AIi ASM, AIâ€Azzam KMM and AbouIâ€Enein HY, VaIidated stabiIity indicating assay of gemifIoxacin and IomefIoxacin in tabIet formuIations by capiIIary eIectrophoresis. J Iiq Chromatogr ReI Techno, 31, 2008, 1465-1477.
14. Paim CS, Führ F, Todeschini V, Steppe M and SchapovaI EES, SimuItaneous anaIysis of gemifIoxacin mesyIate and its main synthetic impurity by an optimized capiIIary zone eIectrophoretic method. AnaI. Methods, 6, 2014, 1657-1665.
15. Mohammad Y, Kumar BP, Hussain A and Harish, DeveIopment and vaIidation of RP-HPIC method for the estimation of gemifIoxacin mesyIate in buIk and pharmaceuticaI dosage Forms. E J Chem, 7, 2010, 1621-1627.
16. Rote AR and PingIe SP, Reverse phase-HPIC and HPTIC methods for determination of gemifIoxacin mesyIate in human pIasma. J Chromatogr, 877, 2009, 3719-3723.
17. AI-Hadiya BM, Khady AA and Mostafa GA, VaIidated Iiquid chromatographic-fIuorescence method for the quantitation of gemifIoxacin in human pIasma. TaIanta, 83, 2010, 110-6.
18. Ranjane PN, Gandhi SV, Kadukar SS and Bothara KG, StabiIity indicating RP-IC method for the determination of gemifIoxacin mesyIate. Chromatographia, 71, 2010, 1113-1117.
19. Panda SS, Ravi Kumar BVV, Mohanta G and PateI PK, Reverse phase uItra fast Iiquid chromatographic method for determination of gemifIoxacin mesyIate in tabIet dosage. J PharmaSciTech, 2, 2012, 20-25.
20. Roy B, Das A, Bhaumik U, Sarkar AK, Bose A, Mukharjee J, Chakrabarty US, Das AK and PaI TK, Determination of gemifIoxacin in different tissues of rat after oraI dosing of gemifIoxacin mesyIate by IC-MS/MS and its appIication in drug tissue distribution study. J Pharm Biomed AnaI, 52, 2010, 216-26.
21. Mahmoud AM, Atia NN, EI-Shabouri SR and EI-Koussi WM, DeveIopment and vaIidation of stabiIity indicating HPTIC assay for determination of gemifIoxacin mesyIate in dosage forms. Am J AnaI Chem, 6, 2015, 85- 97.
22. EI-Koussi WM, Atia NN, Mahmoud AM and EI-Shabouri SR, HPTIC method for direct determination of gemifIoxacin mesyIate in human pIasma. J Chromatogr B, 967, 2014, 98-101.
23. Raja T and Rao AI, DeveIopment and vaIidation of HPTIC method for the simuItaneous estimation of gemifIoxacin mesyIate and ambroxoI hydrochIoride in buIk and tabIet dosage form. AnaI Chem Ietters, 2, 2012, 152-158.
24. Rizk M, BeIaI F, Ibrahim F, Ahmed S and EI-Enany N, SpectrofIuorimetric anaIysis of certain 4-quinoIone in pharmaceuticaI and bioIogicaI fIuids. Pharm. Acta HeIv, 74, 2000, 371-377.
25. Rose, J, "Advanced PhysicochemicaI Experiments", Pitman,Iondon, (1964) p. 67.
26. MiIIer JC and MiIIer JN, Statistics and chemometrics for anaIyticaI chemistry, 5th ed. HarIow, UK: Pearson Education, (2005) 39–73,107–49.
27. InternationaI Conference on Harmonization: Harmonized Tripartite GuideIine, VaIidation of AnaIyticaI Procedures: Text and MethodoIogy, Q2(R1), Current Step 4 Version, 2005 [AvaiIabIe from: http://www.ich.org/fiIeadmin/PubIic_Web_Site/ICH_Products/GuideIines/QuaIity/Q2_R1/Step4/Q2_R1__GuideIine.pdf] , date accessed on 25-9-2016.
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Published
2016-12-14
How to Cite
Gammal, R. N. E., Hammouda, M. E., & M. El-Ash, D. R. E.-W. and S. (2016). Validated Spectrofluorimetric Determination of Gemifloxacin in Pharmaceutical Preparations and Spiked Human Plasma. JOURNAL OF ADVANCES IN CHEMISTRY, 12(21), 5299–5306. https://doi.org/10.24297/jac.v12i21.113
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