IJMST 2018 Volume 8 Issue 2

International Journal of Medical Sciences and Technology (IJMST) ISSN:0974-5343

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Farid Abu Shammala. (2018). Comparative Study of Three Spectrophotometric Methods for Diclofenac Quantification in Urine Samples and Pharmaceutical Formulations. International Journal of Medical Sciences and Technology (IJMST) ISSN:0974-5343, 8(2), 11–24. http://doi.org/10.5281/zenodo.1665833

Title:

Comparative Study of Three Spectrophotometric Methods for Diclofenac Quantification in Urine Samples and Pharmaceutical Formulations

Authors & Affiliation:

Farid Abu Shammala

Assistant Professor, Faculty of Pharmacy, University of Palestine , El-Zahra City, Gaza, PALESTINE

drfaridshammala@hotmail.com

Abstract

This paper reports a comparative study between three spectrophotometric methods for determining the concentration of diclofenac (DCF) in urine samples and pharmaceutical formulations. The first method is based on the reaction between diclofenac and tetrachloro-p-benzoquinone (p-chloranil), in methanol medium, measuring absorbance at 535 nm. The second method based on the oxidation of drugs by Fe(III) in the presence of o-phenanthroline, the formation of tris(o-phenanthroline) iron(II) complex (ferroin) measuring absorbance at 510 nm. The third method is based on the reaction of diclofenac (DCF) with potassium permanganate in an alkaline medium, measuring absorbance at 445 nm. For the first method Beer’s law is valid within a concentration range of 1.0–32µgmL-1 for diclofenac sodium. The optimum concentration ranges is 2.0–30 for diclofenac sodium. The molar absorptivities are 1.65  104 L mol-1 cm-1. The limit of detection (LOD) was 1.15x10-5 mol l-1 and the limit of quantification (LOQ) was 2.5x10-5 mol l-1 . The method gave a mean percentage recoveries 99.8±1.2% for diclofenac sodium. For the second method Beer's law is obeyed in a concentration range from of 1.5–35µgmL-1 with a correlation coefficient of 0.9993 and molar absorptivity of 0.50 x103 l mol-1 cm-1. The limit of detection (LOD) was 1.35x10-5 mol l-1 and the limit of quantification (LOQ) was 4.49x10-5 mol l-1. The method gave a mean percentage recoveries 99.2±1.5% for diclofenac sodium. For the third method, under optimal conditions, Beer’s law is valid within an optimum concentration ranges of 5-50µgmL-1 for diclofenac sodium. The optimium concentration range is 10.0 to 100µgmL-1, with a detection limit of 2.15x10-5 mol l-1 and the limit of quantification (LOQ) was 5.69x10-5 mol l-1. The method gave a mean percentage recoveries 99.5±2.3% for diclofenac sodium. Thus, first method is most accurate method determination of total diclofenac (DCF) in urine samples and pharmaceutical formulations.