Analytical Sciences

Abstract − Analytical Sciences, 35(11), 1183 (2019).

Investigation of a New Spectrophotometric Method for the Analysis of Ciprofloxacin Based on Microwave Assisted Diazotization
Zahid HUSSAIN,*1 Nadia BASHIR,*2 Hussain GULAB,*3 Muhammad ASIM,*2 Khalid M. KHAN,*4 and Shahnaz PERVEEN*5
*1 Department of Chemistry, Abdul Wali Khan University Mardan, 23200, Pakistan
*2 Department of Chemistry, Hazara University, Mansehra, Pakistan
*3 Department of Chemistry, Bacha Khan University, Charsadda, Pakistan
*4 H. E. J. Research Institute of Chemistry, International Centre for Chemical and Biological Sciences, University of Karachi, Karachi-75270, Pakistan
*5 PCSIR Laboratoires Complex, Karachi, Shahrah-e-Dr. Salimuzzaman Siddique, Karachi-75280, Pakistan
A microwave-assisted diazotization reaction of ciprofloxacin was used for the analysis of ciprofloxacin in pharmaceutical samples. The ciprofloxacin was diazotized with phenol using acidified sodium nitrite in a domestic microwave oven. Faster microwave heating and microwave effects were found to be very effective for the process of diazotization. The microwave-assisted reaction was initiated in an acidic media and the colored product was stabilized in a slightly basic medium using a NaOH solution as a neutralizer. The product was found to exhibit the maximum absorbance at 440 nm. All of the experimental conditions like the concentration of reagents, microwave power and reaction time were optimized. The optimum concentrations for phenol, sodium nitrite, HCl and NaOH were found to be 140 ppm, 300 ppm, 0.006 M and 0.006 M respectively. The optimum reaction time was found to be 2 min and a medium high power of the microwave was found to be most effective. The limit of detection (LOD) and the limit of quantification (LOQ) were found to be 1.08 and 3.61 mg L−1 respectively. The developed method was successfully applied for the determination of ciprofloxacin in pharmaceutical samples. This new spectrophotometric method for the analysis of ciprofloxacin is fast, sensitive, easy and cost effective.