Development and Validation of an LC-MS/MS-ESI Method for Comparative Pharmacokinetic Study of Ciprofloxacin in Healthy Male Subjects.
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(r2>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.
Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India.
Hira
H
Choudhury
Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India.
Bapi
B
Gorain
Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India.
Anwesha
A
Paul
Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India.
Pradipta
P
Sarkar
Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India.
Shubhasis
S
Dan
Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India.
Pragnya
P
Chakraborty
Department of Pharmaceutical Technology, Bioequivalence Study Centre, Jadavpur University, Kolkata, India.
Tapan K
TK
Pal
D002138:Calibration; D002853:Chromatography, Liquid / Q000379:methods* / Q000592:standards; D002939:Ciprofloxacin / Q000097:blood / Q000493:pharmacokinetics*; D018592:Cross-Over Studies; D004355:Drug Stability; D006801:Humans; D059625:Liquid-Liquid Extraction; D008297:Male; D012680:Sensitivity and Specificity; D021241:Spectrometry, Mass, Electrospray Ionization / Q000379:methods* / Q000592:standards*; D053719:Tandem Mass Spectrometry / Q000379:methods* / Q000592:standards*; D013810:Therapeutic Equivalency
D002939:Ciprofloxacin