RAPID AND VALIDATED HPLC-UV METHOD FOR DETERMINATION OF GEMIFLOXACIN IN HUMAN URINE

Authors

  • Dalia Zidan Aga Health Insurance Hospital, Dakahlia
  • Omnia A. Ismaiel Department of Analytical Chemistry, Faculty of Pharmacy, Zagazig University
  • Wafaa S. Hassan Zagazig University
  • Abdalla Shalaby Zagazig University

Keywords:

Gemifloxacin, RP-HPLC, Human urine

Abstract

Objective: To develop and validate a simple and rapid reversed phase high performance liquid chromatographic (RP-HPLC) method for the determination of Gemifloxacin (GFX) in human urine.

Methods: GFX was isolated from urine samples after acidification using methylene chloride. Good chromatographic separation was achieved using C18 Ultrasphere (250 mm × 4.6 mm, 5 µm.) analytical column maintained at 25 °C. The mobile phase consisted of methanol and 0.1 M phosphate buffer pH 3 in the ratio of (48: 52, v/v), respectively. The analysis time was 10 min at a 1.0 ml/min flow rate. The UV detection was carried out at 272 nm.

Results: GFX has been eluted at 7.5 min. Linearity was obtained over a concentration range of 20-200 ng/ml (r2>0.999). The extraction recovery of GFX from urine samples was 60%. The proposed method demonstrated excellent intra-and inter-day precision and accuracy within 1.19% and 100.65 %, respectively. The limit of detection (LOD) was found to be 6.3 ng/ml.

Conclusion: Simple and accurate RP-HPLC method for determination of GFX in human urine was developed and validated. The method was successfully applied for determination of GFX in human urine samples from healthy volunteers up to 24 hours after oral administration of 320 mg gemi floxacin tablets.

 

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References

Sweetman S, Blake P, McGlashan J, Neathercoat G, Parsone A. Martindal the complete drug reference. 36th ed. London. UK: Pharmaceutical Press: Sean Sweetman; 2009.

Kadi AA, Angawi RF, Attwa MW, Darwish HW, Abdelhameed AS. High throughput quantitative bioanalytical LC/MS/MS determination of Gemifloxacin in human urine. J Chem 2013. doi.org/10.1155/2013/905704. [Article in Press].

Johnson D, Jones R, Erwin M, Center VM, Institute CM, AccuMed C, et al. Anti-streptococcal activity of SB-265805 (LB20304), a novel fluoronaphthyridone, compared with five other compounds, including quality control guidelines. Diagn Microbiol Infect Dis 1999;33(2):87-91.

Lopez H, Stepanik D, Vilches V, Scarano S, Sarachian B, Mikaelian G, et al. Comparative in vitro activity of Gemifloxacin against gram-positive and gram-negative clinical isolates in Argentina. Diagn Microbiol Infect Dis 2001;40(4):187-92.

Blondeau J, Tillotson G. Gemifloxacin for the treatment of uncomplicated urinary infections (acute cystitis). Ginecol Obstet Mex 2009;77(12):573-82.

Davies TA, Kelly LM, Pankuch GA, Credito KL, Jacobs MR, Appelbaum PC. Antipneumococcal activities of Gemifloxacin compared to those of nine other agents. Antimicrob Agents Chemother 2000;44(2):304-10.

Abbanat D, Macielag M, Bush K. Novel antibacterial agents for the treatment of serious Gram-positive infections. Expert Opin Invest Drugs 2003;12(3):379-99.

Öncü S. Treatment of community-acquired pneumonia, with special emphasis on Gemifloxacin. Ther Clin Risk Manage 2007;3(3):441.

Blondeau JM. Fluoroquinolones: mechanism of action, classification, and development of resistance. Surv Ophthalmol 2004;49(2):S73-S8.

Hassan SS, Hayat U, Tariq I, Ahmad I, Hayat MM, Uzair M, et al. Spectrophotometric method for the determination of Gemifloxacin mesylate in pure and tablet dosage form. Pak J Pharm Sci 2014;27(5):1171-4.

Ambadas RR, Sunita PP. Validated UV-spectrophotometric methods for determination of Gemifloxacin mesylate in pharmaceutical tablet dosage forms. J Chem 2010;7(S1):S344-S8.

Gouda AA, Amin AS, El-Sheikh R, Yousef AG. Spectrophotometric determination of Gemifloxacin mesylate, moxifloxacin hydrochloride, and enrofloxacin in pharmaceutical formulations using acid dyes. J Anal Methods Chem 2014;286379(10):22.

Sahu S, Patro SK, Narayan UL, Garnaik B. Ion-pair spectrophotometric estimation of Gemifloxacin. Pharm Methods 2012;3(1):26-30.

Tekkeli SEK, Önal A. Spectrofluorimetric methods for the determination of Gemifloxacin in tablets and spiked plasma samples. J Fluoresc 2011;21(3):1001-7.

Charan DC, Satyabrata S. Simple and rapid spectrophotometric estimation of Gemifloxacin mesylate in bulk and tablet formulations. Int J PharmTech Res 2011;3(1):133-5.

Paim CS, Führ F, Steppe M, Schapoval EES. Gemifloxacin mesylate: UV spectrophotometric method for quantitative determination using experimental design for robustness. Quimica Nova 2012;35(1):193-7.

Krishna MV, Sankar DG. Spectrophotometric determination of Gemifloxacin mesylate in pharmaceutical formulations through ion-pair complex formation. J Chem 2008;5(3):515-20.

Xia Q, Yang Y, Liu M. Spectrofluorimetric determination of fluoroquinolones in honey with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone in the presence of beta-cyclodextrin. J Fluoresc 2013;23(4):713-23.

Ebraheem SA, Elbashir AA, Aboul-Enein HY. Spectrophotometric methods for the determination of Gemifloxacin in pharmaceutical formulations. Acta Pharm Sin B 2011;1(4):248-53.

Elbashir AA, Saad B, Salhin Mohamed Ali A, Alâ€Azzam KM, Aboulâ€Enein HY. Validated stability indicating assay of Gemifloxacin and lomefloxacin in tablet formulations by capillary electrophoresis. J Liq Chromatogr Relat Technol 2008;31(10):1465-77.

Kaiser M, Grunspan LD, Costa TD, Tasso L. Reversed phase liquid chromatography method with fluorescence detection of Gemifloxacin in rat plasma and its application to the pharmacokinetic study. J Chromatogr B: Anal Technol Biomed Life Sci 2011;879(30):3639-44.

Al-Hadiya BM, Khady AA, Mostafa GA. Validated liquid chromatographic-fluorescence method for the quantitation of Gemifloxacin in human plasma. Talanta 2010;83(1):110-6.

Rote AR, Pingle SP. Reverse phase-HPLC and HPTLC methods for determination of Gemifloxacin mesylate in human plasma. J Chromatogr B Analyt Technol Biomed Life Sci 2009;877(29):3719-23.

Sultana N, Shamim S, Gul MAS, Arayne MS. Simultaneous determination of Gemifloxacin and diuretics in bulk, pharmaceutical dosage forms and human serum by RP-HPLC. Quimica Nova 2010;33(7):1590-3.

Sultana N, Arayne MS, Shamim S, Akhtar M, Gul S. Validated method for the determination of Gemifloxacin in bulk, pharmaceutical formulations and human serum by RP-HPLC: in vitro applications. J Braz Chem Soc 2011;22(5):987-92.

Lee W, Hong CY. Direct liquid chromatographic enantiomer separation of new fluoroquinolones including Gemifloxacin. J Chromatogr A 2000;879(2):113-20.

Gumustas M, Ozkan SA. Simple, sensitive and reliable LC-DAD method of Gemifloxacin determination in pharmaceutical dosage forms. Turk J Pharm Sci 2012;9(2):161-70.

de Araujo BV, Laureano JV, Grunspan LD, Dalla Costa T, Tasso L. Validation of an efficient LC-microdialysis method for Gemifloxacin quantitation in lung, kidney and liver of rats. J Chromatogr B: Anal Technol Biomed Life Sci 2013;920:62-6.

Nageswara Rao R, Naidu C, Guru Prasad K, Padiya R, Agwane SB. Determination of Gemifloxacin on dried blood spots by hydrophilic interaction liquid chromatography with fluorescence detector: application to pharmacokinetics in rats. Biomed Chromatogr 2012;26(12):1534-42.

Roy B, Das A, Bhaumik U, Sarkar AK, Bose A, Mukharjee J, et al. Determination of Gemifloxacin in different tissues of rat after oral dosing of Gemifloxacin mesylate by LC-MS/MS and its application in drug tissue distribution study. J Pharm Biomed Anal 2010;52(2):216-26.

Doyle E, Fowles SE, McDonnell DF, McCarthy R, White SA. Rapid determination of Gemifloxacin in human plasma by high-performance liquid chromatography-tandem mass spectrometry. J Chromatogr B Biomed Sci Appl 2000;746(2):191-8.

Robledo VR, Smyth WF. A study of the analytical behaviour of selected new molecular entities using electrospray ionisation ion trap mass spectrometry, liquid chromatography, gas chromatography and polarography and their determination in serum at therapeutic concentrations. Anal Chim Acta 2008;623(2):221-30.

Gandhimathi N, Ravi T, Bharathi N. Study of hydrolytic and oxidative behavior of Gemifloxacin mesylate in aqueous solution by LC-MS. JGPT 2010;2:1.

Cho SI, Shim J, Kim M-S, Kim Y-K, Chung DS. On-line sample cleanup and chiral separation of Gemifloxacin in a urinary solution using chiral crown ether as a chiral selector in microchip electrophoresis. J Chromatogr A 2004;1055(1):241-5.

Zhao F, Zhao Wh, Xiong W. Chemiluminescence determination of Gemifloxacin based on diperiodatoargentate (III)â€sulphuric acid reaction in a micellar medium. Luminescence 2013;28(2):108-13.

Al-Mohaimeed AM, Al-Tamimi SA, Alarfaj NA, Aly FA. New coated wire sensors for potentiometric determination of Gemifloxacin in pure form, pharmaceutical formulations and biological fluids. Int J Electrochem Sci 2012;7(12):12518.

US Department of Health and Human Services, Food and Drug Administration; 2001. Available from: http://www.fda.gov/ cder/guidance/4252fnl. htm.

Published

01-07-2015

How to Cite

Zidan, D., O. A. Ismaiel, W. S. Hassan, and A. Shalaby. “RAPID AND VALIDATED HPLC-UV METHOD FOR DETERMINATION OF GEMIFLOXACIN IN HUMAN URINE”. International Journal of Pharmacy and Pharmaceutical Sciences, vol. 7, no. 7, July 2015, pp. 104-8, https://www.innovareacademics.in/journals/index.php/ijpps/article/view/5838.

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