University of Khartoum

New Spectrophotometric and Spectrofluorimetric Methods for the Analysis of Cephalosporins in Pharmaceutical Formulations

New Spectrophotometric and Spectrofluorimetric Methods for the Analysis of Cephalosporins in Pharmaceutical Formulations

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Title: New Spectrophotometric and Spectrofluorimetric Methods for the Analysis of Cephalosporins in Pharmaceutical Formulations
Author: Shazalia Mahmoud Ali, Ahmed
Abstract: The objective of this research is to study the optimization, validation, and application of spectrophotometry and spectrofluorimety for the determination of some cephalosporins namely cephalexin (ceph), cefixime (cefi), cefotaxime sodium (cefo), cefadroxil (cefa) and cefuroxime sodium (cefu) in their pharmaceutical formulations. In this work, four simple, rapid, accurate and sensitive spectrophotometric and spectrofluorimetric methods have been developed. The first method (A) is a direct spectrophotometric method based on the reaction between ceph, cefi, cefo, cefa and cefu; with 1, 2-naphthoquinone-4-sulphonate (NQS) reagent. In alkaline medium, an orange-colored products exhibiting maximum absorption peak (_5;max) at 455, 520, 493, 470 and 460 nm for ceph, cefi, cefo, cefa and cefu, respectively were produced. Under the optimized reaction conditions, Beer’s law correlating the absorbance (Y) with concentration (X) was obeyed in the range of 0.8-2.8, 0.5-3, 0.2-1.2, 1-6 and 0.1-0.6 µg/mL for ceph, cefi, cefo, cefa and cefu, respectively. The second method (B) is spectrofluorimetric method based on the reaction of the studied drugs with (NQS) and the extraction of the fluorescent products in chloroform, the fluorescent intensities of the extracted products were measured at 580, 600, 580, 610 and 605 nm and at 455, 520, 490, 470 and 460 nm after excitation for ceph, cefi, cefo, cefa and cefu, respectively. Beer’s law was obeyed in the range 10-60, 10-35, 20-45, 20-70 and 15-40 ng/mL for ceph, cefi, cefo, cefa and cefu, respectively. The third method (C) is a direct spectrophotometric method based on the reaction between ceph, cefi, cefo, cefa and cefu with 8-hydroxy-1, 3, 6- pyrenetrisulfonate trisodium salt, (HPTS). In alkaline medium, a green- colored products exhibiting maximum absorption peak (_5;max) at 470, 480, 479, 485 and 475 for ceph, cefi, cefo, cefa and cefu, respectively were produced. Beer’s law was obeyed in the range 0.3-1.8, 0.1-0.6, 0.5-3, 1-6 and 0.5-3 µg/mL for ceph, cefi, cefo, cefa and cefu, respectively. The fourth method (D) is spectrofluorimetric method based on the reaction of the studied drugs with (HPTS) and the extraction of the fluorescent products in chloroform, the fluorescent intensities of the extracted products were measured at 500, 520, 510, 600 and 600 nm and at 470, 480, 480, 485 and 475 nm after excitation for ceph, cefi, cefo, cefa and cefu, respectively. Beer’s law was obeyed in the range 5-35, 10-60, 10-60, 1-6 and 15-40 ng/mL for ceph, cefi, cefo, cefa and cefu, respectively. Different variables affecting the reactions were carefully studied and optimized. The four methods were validated with respect to accuracy, precision, linearity, selectivity, sensitivity, limit of detection and limit of quantification according to the International Conference of Harmonization (ICH) guidelines for validation of analytical procedures. They successfully applied to the determination of each drug in its pharmaceutical dosage form with a high accuracy and precision, without interference from the common pharmaceutical additives. The four methods were compared in terms of linear range, limit of detection and limit of quantification it was found that the spectrofluorimetric methods (B and D) offer higher sensitivity and selectivity in comparison with the spectrophotometric methods (A and C). The proposed methods are superior to the previously reported spectrophotometric and spectrofluorimetric methods in terms of their simplicity and sensitivity. They are practical and valuable for the routine application in quality control laboratories for the analysis of the five studied cephalosporins.
Description: 156page
URI: http://khartoumspace.uofk.edu/handle/123456789/13239
Date: 2015-06-16


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