Drug Res (Stuttg) 2017; 67(02): 94-102
DOI: 10.1055/s-0042-116593
Original Article
© Georg Thieme Verlag KG Stuttgart · New York

Development and Validation of an LC-MS/MS-ESI Method for Comparative Pharmacokinetic Study of Ciprofloxacin in Healthy Male Subjects

Hira Choudhury
1   Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India
2   Department of Pharmaceutical Technology, School of Pharmacy, International Medical University, Kuala Lumpur, Malaysia
,
Bapi Gorain
1   Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India
3   Faculty of Pharmacy, Lincoln University College, Kuala Lumpur, Malaysia
,
Anwesha Paul
1   Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India
,
Pradipta Sarkar
1   Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India
,
Shubhasis Dan
1   Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India
,
Pragnya Chakraborty
1   Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India
,
Tapan K. Pal
1   Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India
› Author Affiliations
Further Information

Publication History

received 05 April 2016

accepted 24 August 2016

Publication Date:
07 November 2016 (online)

Abstract

A sensitive, specific and reproducible liquid chromatography coupled to tandem mass spectrometric method was developed and validated for the estimation of ciprofloxacin, an extensively used second-generation quinolone antibiotics, in human plasma. A liquid-liquid extraction of ciprofloxacin and the internal standard, ofloxacin, has been approached from the biological matrix using chloroform. Chromatographic separation was achieved in positive ion modes, isocratically on a 3.5 μm C18 analytical column (75 mm×4.6 mm, i.d.) with 0.2% formic acid solution in water: methanol (10:90, v/v) as mobile phase, at a flow rate of 0.5 mL.min−1. The MS/MS ion transitions were monitored as 332.0→231.3 for ciprofloxacin and 362.2→261.0 for IS. The method showed good linearity in the range of 0.01–5.00 μg.mL−1 (r 2 >0.99) with a good precision (3.37–12.60%) and accuracy (87.25–114%). At the same time, ciprofloxacin was found to be stable during stability studies viz. bench-top, auto-sampler, freeze-thaw cycle and long-term. The developed and validated method was successfully applied to measure plasma ciprofloxacin concentrations in a single dose bioequivalence study.

 
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