Author/Authors :
Lal Maheshwari, Madan Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan , Ali Memon, Ayaz National Centre of Excellence in Analytical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan , Memon, Shahabuddin National Centre of Excellence in Analytical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan , Nisa Memon, Fakhar-un National Centre of Excellence in Analytical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan , Rahman Mughal, Ubed Ur Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan , Dayo, Abdullah Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan , Memon, Naheed Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan , Ghoto, Mohammed Ali Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan , Khan Leghari, M Glaxo Smith Kline Pakistan Limited, 35-Dokyard Road, West Wharf, Karachi 74000, Pakistan
Abstract :
The determination of cefixime 1 has clinical and analytical importance due to its broad spectrum antimicrobial activity and stability. Cefixime is a significant member of orally active third generation cephalosporin and has excellent activity against many pathogens. It is for first time that we have developed a new HPLC–DAD method for analysis of imine derivative 3 of cefixime by using reflux method at 100 C for 50 min without any buffer solution. 2 Thiophenecarboxaldehyde (2TCA)
2 was used first time as a derivatizing reagent for cefixime drug. Furthermore, separation of three components,
i.e. drug (cefixime), reagent (2TCA) and derivative was carried out using kromasil 100 C-18 (15 mm · 0.46 mm, 5 lm) column with isocratic elution of methanol: 0.1% aqueous formic acid (70:30 v/v) with flow rate of 1 ml min1 at retention time of 1.8, 2.4 and 3.3 min, respectively; while, total run time was 5 min. The developed method was repeatable with a relative standard deviation (RSD) of 0.81–1.88% for imine derivative. The limit of detection and quantification of imine derivative 3 were obtained within the range of 0.132–0.401 lg ml1 and compared with cefixime drug as 0.30– 0.90 lg ml1, respectively. However, the formation of imine derivative 3 was confirmed by comparing peak height, retention time and spectral changes. The method is rapid, simple, very stable and accurate for the separation and determination of imine derivative 3 of cefixime 1.
