title: Sensitive spectrophotometric determination of aceclofenac following azo dye formation with 4-carboxyl-2,6-dinitrobenzene diazonium ion.
abstract: The study is a description of a sensitive spectrophotometric determination of aceclofenac following azo dye formation with 4-carboxyl-2,6-dinitrobenzenediazonium ion (CDNBD). Spot test and thin layer chromatography revealed the formation of a new compound distinct from CDNBD and aceclofenac. Optimization studies established a reaction time of 5 min at 30 degrees C after vortex mixing the drug/CDNBD for 10 s. An absorption maximum of 430 nm was selected as analytical wavelength. A linear response was observed over 1.2-4.8 μg/mL of aceclofenac with a correlation coefficient of 0.9983 and the drug combined with CDNBD at stoichiometric ratio of 2 : 1. The method has a limit of detection of 0.403 μg/mL, limit of quantitation of 1.22 μg/mL and is reproducible over a three day assessment. The method gave Sandell's sensitivity of 3.279 ng/cm2. Intra- and inter-day accuracies (in terms of errors) were less than 6% while precisions were of the order of 0.03-1.89% (RSD). The developed spectrophotometric method is of equivalent accuracy (p > 0.05) with British Pharmacopoeia, 2010 potentiometric method. It has the advantages of speed, simplicity, sensitivity and more affordable instrumentation and could found application as a rapid and sensitive analytical method of aceclofenac. It is the first described method by azo dye derivatization for the analysis of aceclofenac in bulk samples and dosage forms.
authors.affiliation: Department of Pharmaceutical Chemistry, Faculty of Pharmacy, University of Ibadan, Orita UI, Ibadan, Nigeria.
authors.forename: Segun A
authors.initials: SA
authors.lastname: Aderibigbe
authors.forename: Olajire A
authors.initials: OA
authors.lastname: Adegoke
authors.forename: Olakunle S
authors.initials: OS
authors.lastname: Idowu
authors.forename: Sefiu O
authors.initials: SO
authors.lastname: Olaleye
mesh_terms: D000894:Anti-Inflammatory Agents, Non-Steroidal / Q000032:analysis*; D003979:Diazonium Compounds / Q000737:chemistry*; D004008:Diclofenac / Q000031:analogs & derivatives* / Q000032:analysis; D012680:Sensitivity and Specificity; D013053:Spectrophotometry / Q000379:methods*; D013607:Tablets
chemical_list: C504881:4-carboxyl-2,6-dinitrobenzenediazonium ion; D000894:Anti-Inflammatory Agents, Non-Steroidal; D003979:Diazonium Compounds; D013607:Tablets; D004008:Diclofenac; C056498:aceclofenac