Olakunle S. Idowu

A new spectrophotometric method for the determination of nadolol

A new spectrophotometric method has been developed for the assay of nadolol in pure form and in tablets. The assay procedure is based on a derivatization methodology employing 4-carboxyl-2,6-dinitrobenzene diazonium ion (CDNBD) as a diazo coupling reagent. The azo dye formed between nadolol and CDNBD absorbed visible light at the wavelength maximum of 416 nm (λmax) demonstrating a bathochromic shift from the absorption maximum of nadolol. Optimization studies established an optimal reaction time of 10 min at 60 °C. The assays were linear over 1.25–10 μg ml−1 of nadolol, and the reaction occurred by a 3:1 reagent/drug stoichiometric ratio. The method is found to be selective and has a lower detection limit of 0.29 μg ml−1. Recovery studies over three days gave mean recovery of 101.4% (RSD 3.0%). This new method has been successfully applied in the determination of nadolol and nadolol/bendroflumethiazide tablets with accuracy and precision similar to the official (USP) HPLC procedure (p > 0.05). The new procedure has the advantages of high sensitivity, lower limit of detection and could find application as an in-process quality control method for nadolol.

A new colorimetric method for the determination of nifedipine tablets by derivatization using 4-carboxyl-2,6-dinitrobenzene diazonium ion

BackgroundA new sensitive colorimetric determination of nifedipine has been developed following azo dye formation with 4-carboxyl-2,6-dinitrobenzenediazonium ion (CDNBD). Judging from the various generic brands currently now available, this research was conceived as a means of developing an alternative cost-effective and readily adaptable method for the assay of nifedipine in tablets and for which official high performance liquid chromatographic technique may not be readily available.ResultsNifedipine was reduced with Zn/HCl reduction system and then the diazo coupling reaction was carried out with the CDNBD reagent to generate a new azo adduct with optimal wavelength at 470 nm representing a bathochromic shift relative to nifedipine, reduced nifedipine and CDNBD reagent. Optimal temperature and time for coupling were selected as 50 oC and 15 minutes. A linear response was observed over 2.9 -14.5 µg/mL of nifedipine with a correlation coefficient of 0.9985 and the drug combined with CDNBD at a stoichiometric ratio of 2:1. The method has limits of detection and quantitation of 0.1344 µg mL-1 and 0.4074 µg mL-1 respectively. The Sandell’s sensitivity obtained is 4.673 ng/cm2 and the method was reproducible over a three day assessment. Intra- and inter-day accuracies (in terms of errors) were of the order -0.008 to 3.22 % while precisions were generally less than 3.1 % (RSD).ConclusionsThe developed spectrophotometric method is of equivalent accuracy (p > 0.05) with USP 2007 HPLC method. It has the advantages of speed, simplicity, sensitivity and more affordable instrumentation and could find application as a rapid and sensitive analytical method for nifedipine. It is the first described method by azo dye derivatization for the analysis of nifedipine in bulk samples and dosage forms.