Akram M. El-Didamony

Spectroscopic, structure and antimicrobial activity of new Y(III) and Zr(IV) ciprofloxacin.

The preparation and characterization of the new solid complexes [Y(CIP)2(H2O)2]Cl(3)·10H2O and [ZrO(CIP)2Cl]Cl·15H2O formed in the reaction of ciprofloxacin (CIP) with YCl3 and ZrOCl(2)·8H2O in ethanol and methanol, respectively, at room temperature were reported. The isolated complexes have been characterized with elemental analysis, IR spectroscopy, conductance measurements, UV-vis and 1H NMR spectroscopic methods and thermal analyses. The results support the formation of the complexes and indicate that ciprofloxacin reacts as a bidentate ligand bound to the metal ion through the pyridone oxygen and one carboxylato oxygen. The activation energies, E*; entropies, ΔS*; enthalpies, ΔH*; Gibbs free energies, ΔG*, of the thermal decomposition reactions have been derived from thermogravimetric (TGA) and differential thermogravimetric (DTG) curves, using Coats-Redfern and Horowitz-Metzeger methods. The proposed structure of the two complexes was detected by using the density functional theory (DFT) at the B3LYP/CEP-31G level of theory. The ligand as well as their metal complexes was also evaluated for their antibacterial activity against several bacterial species, such as Staphylococcus aureus (S. aureus), Escherichia coli (E. coli) and Pseudomonas aeruginosa (P. aeruginosa) and antifungal screening was studied against two species (Penicillium (P. rotatum) and Trichoderma (T. sp.)). This study showed that the metal complexes are more antibacterial as compared to free ligand and no antifungal activity observed for ligand and their complexes.

Utilization of oxidation reactions for the spectrophotometric determination of captopril using brominating agents.

Three simple, accurate and sensitive methods (A-C) for the spectrophotometric assay of captopril (CPL) in bulk drug, in dosage forms and in the presence of its oxidative degradates have been described. The methods are based on the bromination of captopril with a solution of excess brominating mixture in hydrochloric acid medium. After bromination, the excess brominating mixture is followed by the estimation of surplus bromine by three different reaction schemes. In the first method (A), the determination of the residual bromine is based on its ability to bleach the indigo carmine dye and measuring the absorbance at 610 nm. Method B, involves treating the unreacted bromine with a measured excess of iron(II) and the remaining iron(II) is complexed with 1,10-phenanthroline and the increase in absorbance is measured at 510 nm. In method (C), the surplus bromine is treated with excess of iron(II) and the resulting iron(III) is complexed with thiocyanate and the absorbance is measured at 478 nm. In all the methods, the amount of bromine reacted corresponds to the drug content. The different experimental parameters affecting the development and stability of the color are carefully studied and optimized. Beers law is valid within a concentration range of 0.4-6.0, 0.4-2.8 and 1.2-4.8 microg mL(-1) for methods A, B and C, respectively. The calculated apparent molar absorptivity was found to be 5.16x10(4), 9.95x10(4) and 1.74x10(5)L mol(-1) cm(-1), for methods A, B and C, respectively. Sandells sensitivity, correlation coefficients, detection and quantification limits are also reported. No interference was observed from common additives found in pharmaceutical preparations. The proposed methods are successfully applied to the determination of CPL in the tablet formulations with mean recoveries of 99.94-100.11% and the results were statistically compared with those of a reference method by applying Students t- and F-test.

Adaptation of a Color Reaction for Spectrophotometric Determination of Diclofenac Sodium and Piroxicam in Pure Form and in Pharmaceutical Formulations

Abstract A simple, sensitive, and convenient spectrophotometric method for the determination of diclofenac sodium and piroxicam in pure form and in pharmaceutical formulations was developed. The method is based on the oxidation of diclofenac sodium or piroxicam by iron(III) in the presence of o‐phenanthroline. The formation of tris(o‐phenanthroline) iron(II) complex (ferroin) upon the reaction of diclofenac sodium or piroxicam with an iron(III)‐o‐phenanthroline mixture in acetate buffer solution of pH 4.4 and 4.8, respectively, was investigated. The ferroin complex is measured at 510 nm against a reagent blank prepared in the same manner. The optimum experimental parameters for the color production are selected. Beers law is valid within a concentration range of 1.0–32 µg mL−1 for diclofenac sodium and 1.0–28 µg mL−1 for piroxicam. For more accurate results, Ringbom optimum concentration ranges are 2.0–30 and 2.0–26 µg mL−1 for diclofenac sodium and piroxicam, respectively. The molar absorptivities are 1.15 × 104 and 1.63 × 104 L mol−1 cm−1, whereas Sandell sensitivities are 2.78 and 2.03 ng cm−2 for diclofenac sodium and piroxicam, respectively. The method gave a mean percentage recoveries 99.8 ± 1.2% for diclofenac sodium and 100.3 ± 0.8% for piroxicam. The developed method is applied for the determination of diclofenac sodium and piroxicam in bulk powder and in their pharmaceutical formulations without any interference from tablet fillers.

A sensitive spectrophotometric method for the determination of propranolol HCl based on oxidation bromination reactions.

Three new, simple, sensitive, rapid and economical spectrophotometric methods (A, B and C) have been developed for the determination of propranolol hydrochloride (PRO) in bulk drug and dosage forms. These methods are based on oxidation-bromination reaction of PRO by bromine, generated in situ by the action of acid on a bromate-bromide mixture, followed by determination of unreacted bromine by three different reaction schemes. In method A, the determination of the residual bromine is based on its ability to bleach the indigo carmine dye and by measuring the absorbance at 610 nm. The residual bromine (in method B), is treated with excess of iron(II) and the resulting iron(III) is complexed with thiocyanate and the absorbance is measured at 480 nm. Method C involves treating the unreacted bromine with a measured excess of iron(II) and the remaining iron(II) is complexed with 1,10-phenanthroline and the increase in absorbance is measured at 510 nm. In all three methods, the amount of bromine reacted corresponds to the drug content. The different experimental parameters affecting the development and stability of the colour are carefully studied and optimized. Beers Law is valid within a concentration range of 1-13, 4-12 and 2-9 µg ml⁻¹ for methods A, B, and C, respectively. The molar absorptivity, Sandells sensitivity, detection and quantification limits are calculated. Common excipients used as additives in pharmaceutical preparations do not interfere in the proposed methods. The proposed methods have been successfully applied to the determination of PRO in pharmaceutical preparations and the results were statistically compared with those of the official method by applying the Students t-test and F-test.

Spectrophotometric Determination of Sparfloxacin in Pharmaceutical Preparations by Ternary Complex Formation with Pd(II) and Eosin

Abstract A simple, sensitive, and direct spectrophotometric method has been developed for the assay of sparfloxacin in bulk and pharmaceutical preparations. The proposed method is based on the formation of ternary complex between an investigated drug, palladium(II) ion and eosin in the presence of methylcellulose as surfactant and acetate buffer of pH 4.2. Spectrophotometrically, under the optimum conditions, the ternary complex showed absorption maximum at 550 nm, with apparent molar absorptivity of 2.69×104 l mol−1 cm−1, Sandells sensitivity of 0.01458 µg ml−1 and linearity in the concentration range 1.6–16 µg ml−1. The composition of the ternary complex was studied by Jobs method of continuous variation and the result indicated that the molar ratio of SPFX: Pd: eosin is 1∶1∶1. The optimum reaction conditions and other analytical parameters are evaluated. The proposed method was successfully applied for the determination of SPFX in its pharmaceutical product with mean percentage recoveries of 99.71%. The observed data has been subjected to statistical analysis, which revealed high accuracy and precision.

Indirect spectrophotometric determination of gentamicin and vancomycin antibiotics based on their oxidation by potassium permanganate

Four simple, accurate, sensitive and economical procedures (A–D) for the estimation of gentamicin sulphate and vancomycin hydrochloride, both in pure form and in pharmaceutical formulations have been developed. The methods are based on the oxidation of the studied drugs by a known excess of potassium permanganate in sulphuric acid medium and subsequent determination of unreacted oxidant by reacting it with amaranth dye (method A), acid orange II (method B), indigocarmine (method C) and methylene blue (method D), in the same acid medium at a suitable λmax=521, 485, 610 and 664 nm, respectively. The reacted oxidant corresponds to the drug content. Regression analysis of Beer-Lambert plots showed good correlations in the concentration ranges 4–8, 3–8, 4–9 and 5–9 µg ml−1 with gentamicin and 4–8, 1.5–4, 1.5–4 and 3.5–5.5 µg ml−1 with vancomycin for methods A, B, C, and D, respectively. The molar absorptivity, sandell sensitivity, detection and quantification limits were calculated. The stoichiometric ratios for the cited drugs were studied. The optimum reaction conditions and other analytical parameters were evaluated. The influence of the substance commonly employed as excipients with these drugs were studied. The proposed methods were applied to the determination of these drugs in pharmaceutical formulations. The results have demonstrated that the methods are equally accurate and reproducible as the official methods.

Extractive Spectrophotometric Method for the Determination of Some Antipsychotic Drugs Using Eriochrome Black T

Simple, accurate, precise, and rapid extractive spectrophotometric method was developed for the determination of four antipsychotics drugs, namely sulpiride (SUP), olanzapine (OLP), clozapine (CLP) and aripiprazole (ARP) both in tablets and in biological fluids. The method was based on the formation of red colored ion-pair complex between the studied drugs and eriochrome black T (EBT) with absorption maxima at 514 nm. The stoichiometry of the complexes in either case was found to be 1: 1 and the conditional stability constant (Kf) of the complexes have been calculated. Reaction conditions were optimized to obtain the maximum color intensity. Beer ’ s law was obeyed in the concentration ranges of 4-30, 4-20, 2-18 and 4-26 µg/ml with SUP, OLP, CLP and ARP, respectively. Various analytical parameters have been evaluated and the results have been validated by satistical data. The proposed method was successfully applied to the analysis of commercial tablets containing the drugs and the results were in good agreement with those obtained with reported methods. The proposed method was further applied to the determination of the studied drugs in spiked human serum and urine. A proposal for the reaction pathway was postulated.

Spectrophotometric Determination of Thioridazine Hydrochloride in Tablets and Biological Fluids by Ion-Pair and Oxidation Reactions

Two simple, sensitive and selective spectrophotometric methods have been described for the determination of the psychoactive drug, thioridazine HCl in tablets and in biological fluids. The first method is based on the oxidation of thioridazine HCl with measured excess of KMnO4 under acidic conditions followed by the determination of unreacted oxidant using indigo carmine and methyl orange. The second method is based on the formation of ion-pair complexes with the acidic sulphophthalein dyes such as bromocresol green and bromocresol purple at pH 1.8 of KCl-HCl buffer. The formed complexes were extracted into methylene chloride and their absorbance was measured at 412 nm. Optimizations of the different experimental conditions are described for both methods. The proposed methods were successfully applied for determination of the drug in tablets and biological fluids with good accuracy and precision. Statistical comparison of the results with those obtained by an official method showed good agreement and indicated no significant difference in accuracy and precision.

Indirect spectrophotometric determination of diltiazem hydrochloride in pure form and pharmaceutical formulations

Three simple, accurate, and sensitive spectrophotometric methods (A, B and C) have been described for the indirect assay of diltiazem hydrochloride (DIL.HCl), either in pure form or in pharmaceutical formulations. The first method (A) is based on the oxidation of DIL.HCl by N-bromosuccinimide (NBS) and determination of unconsumed NBS by measuring the decrease in absorbance of amaranth dye (AM) at a suitable λmax=521 nm. Other methods (B) and (C) involve the addition of excess cerric ammonium sulfate (CAS) and subsequent determination of the unconsumed oxidant by a decrease in the red color of chromotrope 2R (C2R) at a suitable λmax=528 nm or a decrease in the orange-pink color of rhodamine 6G (Rh6G) at λmax=525 nm, respectively. Regression analysis of Beer-Lambert plots showed good correlation in the concentration ranges 3.0–9.0, 3.5–7.0 and 3.5–6.3 μg ml−1 for methods A, B and C, respectively. The apparent molar absorptivity, Sandells sensitivity, detection and quantification limits were calculated. The proposed methods have been applied successfully for the analysis of the drug in its pure form and its dosage form. No interference was observed from a common pharmaceutical adjuvant. Statistical comparison of the results with the reference method shows excellent agreement and indicates no significant difference in accuracy and precision.

Spectrophotometric determination of β-adrenergic antagonists drugs via ion-pair complex formation using MO and EBT

Two simple, rapid and sensitive spectrophotometric methods have been proposed for the assay of bisoprolol fumarate (BSF), propranolol hydrochloride (PRH), and timolol maleate (TIM) either in bulk or in pharmaceutical formulations. The methods are based on the reaction of the selected drugs with methyl orange (MO) and eriochrome black T in acidic buffers, after extracting in dichloromethane and measured quantitatively with maximum absorption at 428 and 518 nm for MO and EBT, respectively. The analytical parameters and their effects on the reported systems are investigated. The extracts are intensely colored and very stable at room temperature. The calibration graphs were linear over the concentration range of 0.8–6.4, 0.4–3.6, 0.8–5.6 μg/mL for BSF, PRH, and TIM, respectively, with MO and 0.8–6.4, 0.4–3.2, and 0.8–8.0 μg/mL for BSF, PRH, and TIM, respectively, with EBT. The stoichiometry of the complexes was found to be 1 : 1 in all cases. The proposed methods were successfully extended to pharmaceutical preparations. Excipients used as additive in commercial formulations did not interfere in the analysis. The proposed methods can be recommended for quality control and routine analysis where time, cost effectiveness and high specificity of analytical technique are of great importance.