Polarographic behaviour and determination of paracetamol and salicylamide after treatment with nitrous acid

A polarographic procedure is described for the determination of paracetamol (acetaminophen) and salicylamide after treatment with nitrous acid. The different experimental parameters affecting the derivatization process and the polarographic analysis were studied. The derivatization products were found to be reduced at the dropping mercury electrode over the whole pH range in Britton-Robinson buffers. At pH 7.0, well defined diffusion-controlled cathodic waves were produced for both compounds. Plots of limiting current vs. concentration were linear over the ranges 0.05–0.75 and 0.25–1.5mM for paracetamol and salicylamide, respectively, in the d.c. mode, with minimum detectability of 2.5 × 10^–6 and 1.25 × 10^–5 M, respectively. The procedure was applied to the analysis of some pharmaceutical dosage forms and the results were in good agreement with those obtained by official and compendial methods.     

Macrocyclic Cr3+, Mn2+ and Fe3+ complexes of a mimic SOD moiety: Design,structural aspects,DFT, XRD,optical properties and biological activity

A novel SOD-like macrocycle “H₂DPD” and its trivalent chromium, iron and divalent manganese complexes have been isolated and characterized using the conventional tools. The macrocycle was prepared by 2:2 condensation of P-phenylenediamine with 5,5-dimethyl1,3-cyclohexanedione. IR and electronic spectral data suggested that H₂DPD coordinates to the metal ion as N₄ tetradentate donor with two Cl⁻ occupying the remaining two sites of the distorted octahedron. XRD spectrum of Cr³⁺ complex indicated that the complex crystallizes in a face-centered monoclinic structure with lattice parameters: a = 10.9380 Å; b = 12.4870 Å; c = 12.4600 Å, α = γ = 90° and β = 111.430 with space group P 1 21/c 1 (14). The energy gap (E_HOMO-E_LUMO), molecular electrostatic potential map (EPM) of title compounds, bond length, bond angle, as well as global and local reactivity were estimated using DFT method. The E_g values obtained from electronic spectra of Cr³⁺, Mn²⁺ and Fe³⁺ complexes were found to be 1.284, 1.220 and 1.138 eV, respectively which are in accordance with those evaluated by DFT revealing semiconductor nature. Also, the thermal degradation of all title compounds was carried out and the kinetic parameters were evaluated using Coats-Redfern and Horowitz-Metzger equations. Moreover, the compounds have screened for antibacterial as well as superoxide mimic activities. Cr³⁺ complex exhibited the most significant potent activity against all bacterial strains. With respect to SOD-like activity, the macrocycle showed the most remarkable SOD-like activity comparable to the standard drug, ascorbic acid.     

Spectrophotometric determination of acyclovir and ribavirin in their dosage forms

Two simple, accurate, and reliable spectrophotometric methods have been developed for the determination of 2 antiviral drugs, acyclovir (ACV) and ribavirin (RBV), in their pharmaceutical formulations. These methods are based on oxidation of the 2 drugs with either cerium (IV) ammonium sulfate (Method A) or potassium persulfate (Method B). The products of oxidation in both methods are coupled with 3-methylbenzothiazolin 2-one hydrazone, producing a deep blue color with a maximum absorption wavelength at 630 nm. In Method A, the absorbance-concentration plots were linear over the ranges of 5-50 and 10-60 microg/mL with detection limits of 0.18 microg/mL (8 x 10(-7) M) and 0.63 microg/mL (2.58 x 10(-6) M) for ACV and RBV, respectively. In Method B, the ranges were 5-45 and 20-50 microg/mL with detection limits of 0.11 microg/mL (4.88 x 10(-7) M) and 1.40 microg/mL (5.73 x 10(-6) M) for the 2 drugs, respectively. The molar absorptivities were 4.1 x 10(3) and 3.65 x 10(3) L/mol/cm in Method A and 5.03 x 10(3) and 3.97 x 10(3) L/mol/cm in Method B for the 2 drugs, respectively. The proposed methods were applied successfully for the determination of the 2 drugs in their pharmaceutical formulations. The percentage recoveries +/- standard deviation were 99.57 +/- 0.86 and 100.82 +/- 0.46 for ACV; 99.41 +/- 1.08 and 100.35 +/- 1.03 for RBV. The results obtained were compared statistically with those given by official methods and showed no significant differences regarding accuracy and precision.     

Second-Derivative Synchronous Fluorescence Spectroscopy for the Simultaneous Determination of Fluphenazine Hydrochloride and Nortriptyline Hydrochloride in Pharmaceutical Preparations

A rapid, simple, and highly sensitive second-derivative synchronous fluorimetric (SDSF) method has been developed for the simultaneous analysis of binary mixtures of fluphenazine hydrochloride (FLZ) and nortriptyline hydrochloride (NTP) in their co-formulated tablets. The method is based upon measurement of the native fluorescence of these drugs at constant wavelength difference (Δλ)?=?120 nm in acetic acid. The different experimental parameters affecting the fluorescence intensity of the studied drugs were carefully studied and optimized. The fluorescence-concentration plots were rectilinear over the range of 0.25–3.0 and 1–10 μg/ml for FLZ and NTP respectively, with lower detection limits (LOD) of 0.05 and 0.18 μg/ml and quantitation limits of 0.15 and 0.53 μg/ml for FLZ and NTP respectively. The proposed method was successfully applied for the determination of the studied compounds in their synthetic mixtures and in commercial co-formulated tablets. The results obtained were in good agreement with those obtained by the reference methods.     

Spectrophotometric determination of chlordiazepoxide and nitrazepam

The use of ethyl acetoacetate in the spectrophotometric determination of chlordiazepoxide and nitrazepam has been investigated. The procedure is based on coupling the diazotized drugs with ethyl acetoacetate, which possesses an active methylene group. The products have absorption maxima at 408 and 482 nm and apparent molar absorptivities of 2.74 x 10(4) and 4.11 x 10(4) 1.mole(-1).cm(-1), respectively. The method is simple, highly sensitive and suitable for 1-16 mug/ml concentrations of the two compounds, with mean recoveries of 100.3 +/- 1.2 and 99.8 +/- 1.0% respectively.     

2-Iodylbenzoic acid as an oxidizing agent for the determination of certain thioxanthene derivatives

An indirect titrimetric method is described for the determination of chlorprothixene, methixene and thiothixene. A known and excessive volume of 2-iodylbenzoate is added and after a specified time the surplus is determined iodometrically. The method has been applied to the analysis of pharmaceutical preparations containing these drugs and the results obtained compare favourably with those from the pharmacopoeial methods. The method is simple, accurate and precise.     

Spectrofluorometric determination of ketorolac tromethamine via its oxidation with cerium(IV) in pharmaceutical preparations and biological fluids

A simple and sensitive fluorometric method for determination of ketorolac tromethamine was studied. The method depends on oxidation of the drug with cerium(IV) and subsequent monitoring of the fluorescence of the induced cerium(III) at lambda(em) 365 nm after excitation at 255 nm. Different variables affecting the reaction conditions, such as the concentrations of cerium(IV), sulfuric acid concentration, reaction time, and temperature, were carefully studied and optimized. Under the optimum conditions, a linear relationship was found between the relative fluorescence intensity and the concentration of the investigated drug in the range of 0.1-0.8 microg/mL. No interferences could be observed from the excipients commonly present in dosage forms. The proposed method was successfully applied to the analysis of the investigated drug in its pure form, pharmaceutical preparations, and biological fluids with good accuracy and precision. The recoveries for pharmaceutical formulations ranged from 99.8-101.0 +/- 0.6% for tablets, 98.5-101.0 +/- 1.0% for ampoules, and 99.0-100.5 +/- 0.7% for eye drops. The results obtained by the proposed method were satisfactory compared with those obtained by the official method. The recoveries for biological fluids were 99.1-100.4 +/- 0.7 and 99.0-100.0 +/- 0.5% for plasma and urine, respectively.     

Spectroscopic Determination of Mebendazole Using a 1,10 Phenanthroline–Iron Complex

Journal of Applied Spectroscopy - Simple, rapid, and sensitive spectroscopic methods have been proposed to determine the antifungal drug mebendazole. These methods adapted the reduction of ferric...     

Spectrofluorimetric Determination of Famotidine in Pharmaceutical Preparations and Biological Fluids. Application to Stability Studies

A simple, economic, selective, and stability indicating spectrofluorimetric method was developed for the determination of famotidine (FMT); is based on its reaction with 9, 10-phenanthraquinone in alkaline medium to give a highly fluorescent derivative measured at 560 nm after excitation at 283 nm. The fluorescence intensity - concentration plot was rectilinear over the concentration range of 50–600 ng/ml with minimum quantification limit (LOQ) of 13.0 ng/ml and minimum detection limit (LOD) of 4.3 ng/ml. The factors affecting the development of the fluorescence intensity of the reaction product were carefully studied and optimized. The method was applied for the determination of FMT in its dosage forms. The stability of the compound was studied, and the proposed method was found to be stability indicating one. The results obtained were in good agreement with those obtained by the official method. Furthermore, the method was applied for the determination of FMT in spiked and real human plasma. The mean % recovery (n = 4) was found to be 99.94 ± 0.24, and 105.13 ± 0.64 for spiked and real human plasma, respectively. The composition of the reaction product as well as its stability constant was also investigated. Moreover, the method was utilized to investigate the kinetics of both alkaline and oxidative induced degradation of the drug. The apparent first order rate constant and half life time of the degradation product was calculated. A proposal of the reaction pathway was postulated.     

Colorimetric determination of some important hydrazine derivatives

A simple and rapid colorimetric method for the determination of isoniazid, isocarboxazid, iproniazid phosphate, phenelzine sulphate and phenylhydrazine hydrochloride is described. The method is based on the formation of ferroin, when the studied drugs react with a mixture of iron (III) and 1,10-phenanthroline, and measurement of the absorbance at 512 nm. The procedure has been successfully applied to the assay of the pharmaceutical preparations of the studied drugs and the results are favorably comparable to the official methods.