title: Optimization of HPLC method for determination of cefixime using 2-thiophenecarboxaldehyde as derivatizing reagent: A new approach.
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 μm) column with isocratic elution of methanol: 0.1% aqueous formic acid (70:30 v/v) with flow rate of 1 ml min(-) (1) 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 μg ml(-) (1) and compared with cefixime drug as 0.30-0.90 μg ml(-1), 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.
authors.affiliation: Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan.
authors.forename: Madan Lal
authors.initials: ML
authors.lastname: Maheshwari
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan.
authors.forename: Ayaz Ali
authors.initials: AA
authors.lastname: Memon
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan.
authors.forename: Shahabuddin
authors.initials: S
authors.lastname: Memon
authors.affiliation: National Centre of Excellence in Analytical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan.
authors.forename: Fakhar-Un-Nisa
authors.initials: FU
authors.lastname: Memon
authors.affiliation: Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan.
authors.forename: Ubed Ur Rahman
authors.initials: UU
authors.lastname: Mughal
authors.affiliation: Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan.
authors.forename: Abdullah
authors.initials: A
authors.lastname: Dayo
authors.affiliation: Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan.
authors.forename: Naheed
authors.initials: N
authors.lastname: Memon
authors.affiliation: Faculty of Pharmacy, Department of Pharmaceutical Chemistry, University of Sindh Jamshoro, Sindh 76080, Pakistan.
authors.forename: Mohammed Ali
authors.initials: MA
authors.lastname: Ghoto
authors.affiliation: Glaxo Smith Kline Pakistan Limited, 35-Dokyard Road, West Wharf, Karachi 74000, Pakistan.
authors.forename: M
authors.initials: M
authors.lastname: Khan Leghari
keywords: 2-Thiophenecarboxaldehyde; Cefixime; Derivatization; HPLC–DAD; Reflux method