Nafisur Rahman

Validated spectrophotometric methods for the determination of amlodipine besylate in drug formulations using 2,3-dichloro 5,6-dicyano 1,4-benzoquinone and ascorbic acid

Two simple and sensitive spectrophotometric methods have been proposed for the determination of amlodipine besylate either in pure form or in pharmaceutical formulations. The first method is based on the charge transfer complexation reaction of the drug with 2,3-dichloro 5,6-dicyano 1,4-benzoquinone (DDQ) to give coloured product having maximum absorbance at 580 nm. The second procedure depends on the measurement of purple red colour produced by the interaction of drug with ascorbic acid in N,N-dimethylformamide medium (DMF) which absorbed maximally at 530 nm. Under the optimized experimental conditions, Beers law was obeyed in the concentration ranges of 1-125 and 10-140 microg ml(-1) with DDQ and ascorbic acid, respectively. Both the methods were applied successfully for the analysis of amlodipine besylate in dosage forms. Results of analyses were validated statistically and through recovery studies.

Kinetic spectrophotometric method for the determination of norfloxacin in pharmaceutical formulations

A simple and sensitive kinetic spectrophotometric method is described, based on the oxidation of norfloxacin with alkaline potassium permanganate. The reaction is followed spectrophotometrically by measuring the rate of change of absorbance at 603 nm. The initial rate and fixed time (at 3 min) methods are utilized for constructing the calibration graphs to determine the concentration of the drug. The calibration graphs are linear in the concentration ranges 2.0-20 microg ml(-1) and 1.0-20 microg ml(-1) using the initial rate and fixed time methods, respectively. The results are validated statistically and through recovery studies. The method has been successfully applied to the determination of norfloxacin in commercial dosage forms. Statistical comparison of the results with the reference method shows excellent agreement and indicates no significant difference in accuracy and precision.

Kinetic spectrophotometric method for the determination of ramipril in pharmaceutical formulations.

The objective of this research was to develop a kinetic spectrophotometric method for determination of ramipril in pure form and pharmaceutical formulations. The method was based on the reaction of carboxylic acid group of the drug with a mixture of potassium iodate (KIO3) and potassium iodide (KI) in aqueous medium at room temperature. The reaction is followed spectrophotometrically by measuring the increase in absorbance at 352 nm as a function of time. The initial-rate and fixed-time methods were adopted for constructing the calibration curves. Both the calibration curves were linear in the concentration range of 10.0–70.0 μg mL−1. The detection limits were 0.02μg mL−1 and 0.15-μg mL−1 for initial rate and fixed time methods, respectively. The proposed methods are validated statistically and through recovery studies. The point and interval hypothesis tests have been performed confirming that there is no significant difference between the proposed methods and the reference method. The experimental true bias of all samples is less than ±2%. The methods have been successfully applied to the determination of ramipril in tablets and capsules.

Extractive spectrophotometric methods for determination of diltiazem HCl in pharmaceutical formulations using bromothymol blue, bromophenol blue and bromocresol green

Three simple and sensitive extractive spectrophotometric methods have been described for the assay of diltiazem hydrochloride either in pure form or in pharmaceutical formulations. The developed methods involve formation of coloured chloroform extractable ion-pair complexes of the drug with bromothymol blue (BTB), bromophenol blue (BPB) and bromocresol green (BCG) in acidic medium. The extracted complexes showed absorbance maxima at 415 nm for all three methods. Beers law is obeyed in the concentration ranges 2.5-20.0, 2.5-10.0 and 2.5-12.5 microg ml(-1) with BTB, BPB and BCG, respectively. The methods have been applied to the determination of drug in commercial tablets and capsules. Results of analysis were validated statistically and through recovery studies.

Application of ninhydrin to spectrophotometric determination of famotidine in drug formulations

A simple and fast spectrophotometric procedure has been developed for the determination of famotidine. The method is based on the interaction of ninhydrin with primary amines present in the famotidine. This reaction produces a blue coloured product which absorbed maximally at 590 nm. The effects of variables such as reagent concentration and reaction time were investigated to optimize the procedure. Beers law was obeyed in the concentration range of 5-30 microg ml(-1) with molar absorptivity of 6.99 x 10(3) l M(-1) cm(-1). The results were validated statistically. The proposed method has been applied to the determination of famotidine in tablets with satisfactory results.

Synthesis and characterization of zirconium(IV) iodovanadate and its use as electron exchanger

Samples of zirconium(IV) iodovanadate have been synthesized under varying mixing ratios by adding a mixture of aqueous solution of 0.1 M potassium iodate and 0.1 M sodium metavanadate to aqueous solution of 0.1 M zirconium oxychloride at pH 1. The ion exchange capacity of the material for Na(+) ion was found to be 2.20 meqg(-1) of dry exchanger. The material has been characterized on the basis of chemical composition, FTIR and TGA. The chemical stability of the product has been checked in neutral, acidic and basic media. The product has been used as electron exchanger. The oxidation of Fe(II), Sn(II), ascorbic acid and thioglycolic acid was achieved by batch-equilibrium technique successfully. The maximum redox capacity of the exchanger has been found to be 4.20 meqg(-1) of exchanger by column process.

Optimized and validated spectrophotometric method for the determination of uranium(VI) via complexation with meloxicam

An optimized and validated spectrophotometric method has been developed for the determination of uranyl ion in the presence of other metal ions. The method is based on the chelation of uranyl ion with meloxicam via beta-diketone moiety to produce a yellow colored complex, which absorbs maximally at 398 nm. Beers law is obeyed in the concentration range of 5-60 microg/mL with apparent molar absorptivity and Sandells sensitivity of 5.02 x 10(4)L/mol/cm and 0.1 microg/cm2/0.001 absorbance unit, respectively. The method has been successfully applied for the determination of uranyl ion in synthetic mixture and soil samples. Results of analysis were statistically compared with those obtained by Currahs spectrophotometric method showing acceptable recovery and precision.

Studies on the development of spectrophotometric method for the determination of haloperidol in pharmaceutical preparations

A spectrophotometric method based on the formation of ion-pair complex between haloperidol and eriochrome black T (EBT) at pH 1.85 has been described. The formed complex was extracted quantitatively into chloroform and measured at 510 nm. Infra red (IR) studies were performed to confirm the formation of ion-pair complex. Beer’s law was obeyed in the concentration range of 2.0-9.0 μg mL-1 with molar absorptivity of 2.67 × 104 L mol-1 cm-1. The detection limit was found to be 0.18 μg mL-1. Statistical comparison of the results of the proposed method with those of the reference method shows excellent agreement and indicates no significant difference in accuracy and precision.

Spectrophotometric determination of diltiazem hydrochloride with sodium metavanadate

Abstract A spectrophotometric method for the determination of diltiazem hydrochloride has been developed. The drug is boiled with sodium metavanadate in sulfuric acid medium (11.0 M) for 20 min and the absorbance is measured at 750 nm. Beer’s law is obeyed up to 50 μg ml −1 with R.S.D. of 1.07% and molar absorptivity, 6.18×10 3 l mol −1 cm −1 . The method was applied to the determination of the drug in commercial tablets and capsules.

Quantitative analysis of cefixime via complexation with palladium(II) in pharmaceutical formulations by spectrophotometry

An optimized and validated spectrophotometric method has been developed for the determination of cefixime in pharmaceutical formulations. The method is based on the complexation reaction between cefixime and palladium ion in the presence of acidic buffer solution (pH 3) in ethanol-distilled water medium at room temperature. The complex absorbed maximally at 352 nm. Beer’s law is obeyed in the working concentration range of 2.5–35 μg/mL with apparent molar absorptivity of 1.015×104 L/mol cm and Sandell’s sensitivity of 0.001 μg/cm2/0.001 absorbance unit. The limits of detection and quantitation for the proposed method are 0.175 and 0.583 μg/mL, respectively. The effect of common excipients used as additives has been studied in the determination of cefixime. The proposed method has been successfully applied for the determination of cefixime in pharmaceutical formulations. The results obtained by the proposed method were statistically compared with the reference method using t and F values and found no significant difference between the two methods.