Mohamed H. Abdel-Hay

Colorimetric Determination of Seven Nonsteroidal Antiinflammatory Drugs Using 2-Nitrophenylhydrazine Hydrochloride

Abstract A simple, sensitive and convenient colorimetric method for the determination of seven nonsteroidal anti-inflammatory drugs, namely, flufenamic acid, mefenamic acid, niflumic acid, ketoprofen, ibuprofen, diclofenac sodium and indomethacin, was developed. The method is based on reaction of the abovementioned compounds - being carboxilic compounds, reacting with 2-nitrophenylhydrazine in presence of diclohexylcarbodiimide in ethanolic medium to give acid hydrazine, which showed intense violet colour with a maximum absorption at around 550 nm. The effect of reagent concentration (2-nitrophenylhydrazine hydrochloride, pyridine and dicyclohexylcarbodiimide), heating temperature and heating time were studied to optimize reaction conditions. The method was successfully applied to the determination of those drugs in pure and dosage forms, with a relative standard deviation less than 2%.

Chemical and microbiological investigations of metal ion interaction with norfloxacin

Abstract This report describes a spectrophotometric study on the interaction between norfloxacin (NFX) and metal ions (Al 3+ , Mg 2+ and Ca 2+ ). Two buffers of pH 3.6 and 8.8 were used. A shift in absorption maximum was observed and the stoichiometry of the complex was determined using the Job and molar methods. The ratios were NFX:AL 3+ , 2:1 and 3:1 for the NFX:Mg 2+ complex. The formation of a complex with Al 3+ enhanced the water solubility of the drug. Microbiological studies indicated decreased activity of norfloxacin in the presence of metal ions.

Adsorptive stripping voltammetric behaviour of azomethine group in pyrimidine-containing drugs.

The stripping voltammetric behaviour of buspirone hydrochloride (BUS) and piribedil (PIR), as models of pyrimidine-containing compounds, was studied using a hanging mercury drop electrode (HMDE). A sensitive adsorptive stripping voltammetric method for determination of such drugs is described. The voltammetric peaks were obtained at -1.23 and -1.22 V for BUS and PIR. respectively, which correspond to the reduction of the azomethine group of pyrimidine ring in Britton-Robinson buffer (pH 7). Factors such as pH of supporting electrolyte, accumulation potential and time and instrumental parameters were optimized. Calibration plots and regression data validation, accuracy, precision, limits of detection, limits of quantification, and other aspects of analytical merit are presented. The applicability of the method was evaluated through determination of BUS and PIR in tablet dosage forms. A preliminary study of the analysis of plasma samples, spiked with the investigated drug, after a simple extraction procedure is described.

Spectrofluorimetric determination of guanethidine sulphate, guanoxan sulphate and amiloride hydrochloride in tablets and in biological fluids using 9,10-phenanthraquinone.

A highly sensitive spectrofluorimetric method for the determination of some drugs of the monosubstituted guanidine derivatives in laboratory made tablets, in spiked human serum and in urine samples is presented. The method is based on the reaction of guanethidine sulphate (I), guanoxan sulphate (II) and amiloride hydrochloride (III) with 9,10-phenanthraquinone (IV) to give highly fluorescent derivatives. The linearity ranges were found to be 0.06-0.96 mug/ml for (I) and (II) and 0.04-0.28 mug/ml for (III), with relative standard deviation less than 2%. Mean percentage recoveries for tablets were found to be 99.9 +/- 1.3, 100.5 +/- 1.1 and 100.0 +/- 1.6 for I, II and III, respectively. For I and III the results are highly correlated with the B.P. methods. Using the synchronous fluorimetry, differentiation between I and II was possible. Chloroform, dichloromethane and ethyl acetate have been used to extract I, II and III, respectively from serum and urine at basic pH, followed by applying the proposed fluorimetric method. Percentage recoveries were found to be 95.7-102.2%. The limit of detection is 0.04 mug/ml for I and II and 0.02 mug/ml for III.

Simultaneous Determination of Acetaminophen with Orphenadrine Citrate, Ibuprofen or Chlorzoxazone in Combined Dosage Forms by Zero-Crossing Derivative Spectrophotometry

Abstract A derivative spectrophotmetric procedure for the simultaneous determination of acetaminophen-orphenadrine citrate, acetaminophen-ibuprofen and acetaminophen-chlorzoxazone, binary mixtures is described. The procedure minimises the mutual interference between these drugs in mixtures and allows the determination of these compounds without a previous extraction step. The precision of the method, expressed as the relative standard deviation, is better than 4%. The method has been successfully applied to laboratory mixtures and commercial tablets containing these drugs.

Simultaneous determination of melatonin-pyridoxine combination in tablets by zero-crossing derivative spectrophotometry and spectrofluorimetry.

Two methods have been developed for the analysis of melatonin (M) and pyridoxine hydrochloride (PH) in combination. The first method depends on first- and second-derivative ultraviolet spectrophotometry, with the zero crossing technique of measurement. First-derivative amplitudes at 296 nm and second-derivative amplitudes at 294 and 322 nm are selected for the determination of M and PH, respectively. The second method is based on the native fluorescence of both M and PH, in methanol and 0.1 M hydrochloric acid, respectively, after a preliminary solvent extraction procedure. The relative standard deviation of both methods was less than 2.0%. The two methods have been successfully applied to the determination of both drugs in laboratory-prepared mixtures and in tablets.

Simultaneous determination of theophylline and guaiphenesin by third-derivative ultraviolet spectrophotometry and high-performance liquid chromatography

Two methods are described for the simultaneous determination of theophylline and guaiphenesin in combined pharmaceutical dosage forms. The first method depends on third-derivative ultraviolet spectrophotometry, with the zero crossing technique of measurement. Third-derivative amplitudes at 222 and 278 nm were selected for the assay of guaiphenesin and theophylline, respectively. The second method is based on high-performance liquid chromatography on a reversed-phase column using a mobile phase of 0.01 mol dm-3 sodium dihydrogen phosphate-methanol-acetonitrile (8 + 2 + 1) (pH 5.5) with detection at 245 nm. Both methods showed good linearity, precision and reproducibility. The proposed methods were successfully applied to the determination of these drugs in laboratory-prepared mixtures and in capsules or elixir.

Spectrophotometric Determination of Bisacodyl and Piribedil

ABSTRACT Simple spectrophotometric methods are described for the assay of bisacodyl (BIS) and piribedil (PIR) based on charge‐transfer and ion‐pair complexation reactions. The first method is based on the reaction of the cited drugs with p‐chloranilic acid (p‐CA) in acetonitrile. The purple colored chromogen formed shows maximum absorbance at 518 nm. The second method is concerned with the reaction of the investigated drugs with picric acid (PA) and four sulphonphthalein acid dyes, namely; bromocresol green (BCG), bromocresol purple (BCP), bromophenol blue (BPB) and thymol blue (TB). The yellow ion‐pair complexes formed show absorption spectra with maxima within the range from 400 to 415 nm. The stoichiometric ratio was found to be 1:1, for all complexation reactions examined, as calculated by the continuous variations method. Beers law validation, accuracy, precision, limits of detection, limits of quantification, and other aspects of analytical merit are presented in the text. The proposed methods were applied for the determination of the analytes in their pure forms and in pharmaceutical preparations. The results were in good agreement with those obtained by the official and reported methods.

Colorimetric determination of some penicillins and cephalosporins with 2-nitrophenylhydrazine hydrochloride.

A simple and sensitive calorimetric method for the determination of some penicillins and cephalosporins is presented. The method is based on reaction with 2-nitrophenylhydrazine hydrochloride in presence of dicyclohexylcarbodi-imide and pyridine. The violet colour of the resulting acid hydrazide is measured at the appropriate wavelength. The method has been applied to determination of these antibiotics in bulk and dosage forms, with a coefficient of variation less than 2%.

Sensitive spectrofluorimetric and spectrophotometric methods for the determination of thonzylamine hydrochloride in pharmaceutical preparations based on coupling with dimethylbarbituric acid in presence of dicyclohexylcarbodiimide

Two sensitive and selective spectrophotometric and spectrofluoimetric procedures were developed for the determination of thonzylamine hydrochloride (THAH) in tablets and nasal drops. The methods are based on König reaction which resulted in an orange-yellow fluorescent product. The orange-yellow product of the interaction between the dicyclohexylcarbodiimide (DCC), THAH and dimethylbarbituric acid (DMBA) showed an absorption maximum at 492 nm, a first-derivative signal at 494 nm and a fluorescence emission peak at 518 nm (lambda(ex)=492 nm). The orange-yellow color was found to be stable for at least 2 h. The reaction conditions were studied and optimized. The reaction obeys Beers law over the ranges 8-20 and 0.2-2.0 microg ml(-1) for the derivative spectrophotometric and fluorimetric measurements, respectively. The detection limits were found to be 0.29 and 0.018 microg ml(-1) for the spectrophotometric and fluorimetric measurements, respectively. The proposed methods were applied to the analysis of pharmaceutical formulations containing THAH, either alone or in combination with naphazoline nitrate.