Optimization of HPLC method for determination of cefixime using 2-thiophenecarboxaldehyde as derivatizing reagent: A new approach

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• 作者：Madan Lal Maheshwari^a ; Ayaz Ali Memon^b ; ^{ayazmemon33@gmail.com" class="auth_mail" title="E-mail the corresponding author} ; Shahabuddin Memon^b ; Fakhar-un-Nisa Memon^b ; Ubed Ur Rahman Mughal^a ; Abdullah Dayo^a ; Naheed Memon^a ; Mohammed Ali Ghoto^a ; M. Khan Leghari^c
• 关键词：HPLC&ndash ; DAD ; Reflux method ; Derivatization ; Cefixime ; 2-Thiophenecarboxaldehyde
• 刊名：Journal of the Saudi Pharmaceutical Society
• 出版年：2015
• 出版时间：September 2015
• 年：2015
• 卷：23
• 期：4
• 页码：444-452
• 全文大小：783 K

文摘

The determination of cefixime rong class="boldFont">1rong> 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 rong class="boldFont">3rong> of cefixime by using reflux method at 100 °C for 50 min without any buffer solution. 2 Thiophenecarboxaldehyde (2TCA) rong class="boldFont">2rong> 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 rong class="boldFont">3rong> 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 rong class="boldFont">3rong> 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 rong class="boldFont">3rong> of cefixime rong class="boldFont">1rong>.