Catalytic spectrophotometric determination of iodide in pharmaceutical preparations and edible salt.

The catalytic effect of iodide on the oxidation of four dyes: viz. variamine blue (VB), methylene blue (MB), rhodamine B (RB), and malachite green (MG) with different oxidizing agents was investigated for the kinetic spectrophotometric determination of iodide. The above catalyzed reactions were monitored spectrophotometrically by following the change in dye absorbances at 544, 558, 660, or 617 nm for the VB, RB, MB, or MG catalyzed reactions, respectively. Under optimum conditions, iodide can be determined within the concentration levels 0.064-1.27 µg mL(-1) for VB method, 3.20-9.54 µg mL(-1) for RB method, 5.00-19.00 µg mL(-1) for the MB method, and 6.4-19.0 µg mL(-1) for the MG one, with detection limit reaching 0.004 µg mL(-1) iodide. The reported methods were highly sensitive, selective, and free from most interference. Applying the proposed procedures, trace amounts of iodide in pharmaceutical and edible salt samples were successfully determined without separation or pretreatment steps.

Kinetic catalytic determination of trace levels of iodide based on the oxidation of basic dyes with hydrogen peroxide monitored potentiometrically using simple PVC electrodes.

Four sensitive catalytic potentiometric methods have been developed for trace levels determination of iodide based on its catalytic effects on the oxidation of four dyes: viz. variamine blue (VB), rhodamine B (RB), methylene blue (MB) and malachite green (MG), with H(2)O(2) in H(3)PO(4) medium at 25±0.5°C. The catalyzed reaction rates were estimated potentiometrically by monitoring the potential of the corresponding dye-PVC ion selective electrodes. To select the optimized reaction conditions offering the highest sensitivity of the method, parallel studies were carried out on each dye catalyzed reaction including: the effect of reactant concentration, reaction medium and temperature. The working calibration curves were linear over the concentration range from 0.32 to 2.54 mg L(-1) iodide for VB method and from 3.2 to 12.7 mg L(-1) for other ones. The tolerance limits of more than 20 interfering species were listed indicating the high selectivity of the method. Trace iodide in edible salt and pharmaceutical samples was determined without the need for separation or preconcentration procedures.

Validated polarographic methods for the determination of certain antibacterial drugs.

Two simple, precise, inexpensive and sensitive voltammetric methods for the determination of lomefloxacin (LFX), sparfloxacin hydrochloride (SFX), gatifloxacin (GFX), and moxifloxacin (MFX) were developed. The present methods were first used to explore the adsorption behavior of the four investigated antibacterial agents at a hanging mercury dropping electrode (HMDE), by a direct method and secondly by a modification via their complexation with PdCl(2). For the direct method, drugs were accumulated on HMDE, and a well-defined reduction peak was obtained in Britton-Robinson buffer of pH 7 for LFX and SFX, and pH 6 for GFX and MFX. The adsorptive stripping response was evaluated as a function of some variables such as the scan rate, pH, accumulation time and potential. For the modified method, the adsorptive behavior of Pd(II)-4-quinolone complexes at the HMDE developed a strippining voltammetry peak at a more negative potential than that of the free Pd(II) ions (-1.05 V). The limits of detection (LOD) were 2 x 10(-8) M, while the limits of quantification (LOQ) were 6 x 10(-8) M for the investigated drugs. The methods were applied to the determination of LFX, SFX, GFX, and MFX in biological samples and pharmaceutical preparations, and also compared with the official reference methods. Complete validation of the proposed methods was also done.

Electrochemical adsorptive behavior of some fluoroquinolones at carbon paste electrode.

Cyclic voltammetry and differential pulse voltammetry were used to explore the adsorption behavior of three antibacterial agents at a carbon paste electrode. The drugs were accumulated on a carbon paste electrode, and a well-defined oxidation peak was obtained in acetate buffer (pH 5.0). The adsorptive stripping response was evaluated as a function of some variables such as the scan rate, pH and accumulation time. A simple, precise, inexpensive and sensitive voltammetric method has been developed for the determination of the cited drugs (Lomefloxacin (LFX), Sparfloxacin hydrochloride (SFX), and Gatifloxacin (GFX)). A linear calibration was obtained from 2 x 10(-7) M to 4 x 10(-5) M for LFX, 2 x 10(-7) M to 6 x 10(-5) M for SFX, and GFX. The limits of detection (LOD) were 4.2 x 10(-7), 7 x 10(-7) and 6.6 x 10(-7) M, while the limits of quantification (LOQ) were 1.4 x 10(-6), 2.3 x 10(-6) and 2.2 x 10(-6) M for LFX, SFX, and GFX, respectively. The R. S. D. of five measurements at the 1 x 10(-6) M level were 0.4, 0.5 and 0.3 for LFX, SFX and GFX, respectively. The method was applied to the determination of LFX, SFX and GFX in dilute urine samples and dosage forms, and compared with the HPLC method.

Spectroscopic and voltammetric studies of pefloxacin bound to calf thymus double-stranded DNA.

Spectral and electrochemical studies have been carried out on the interaction of pefloxacin with calf thymus double-stranded dsDNA. The voltammetric behavior of pefloxacin was investigated at glassy carbon, carbon paste and dsDNA-modified carbon paste electrodes using cyclic voltammetry. Pefloxacin was oxidized, yielding one irreversible oxidation peak. The modification of the carbon paste surface with dsDNA allowed an accumulation process to take place for pefloxacin such that higher sensitivity was achieved compared with the bare surface. The response was characterized with respect to ionic strength, accumulation time, pefloxacin concentration, and other variables. The stripping differential pulse voltammetric response showed a linear calibration curve in the range 1.0 x 10(-7)-1.0 x 10(-5) mol l(-1) with a detection limit of 5.0 x 10(-8) mol l(-1) at the dsDNA modified electrode. The method was applied to the direct determination of pefloxacin in diluted urine samples.

A validated stripping voltammetric procedure for quantification of the anti-hypertensive and benign prostatic hyperplasia drug terazosin in tablets and human serum.

The electrochemical behavior of terazosin at the hanging mercury drop electrode was studied in Britton-Robinson buffer (pH 2-11), acetate buffer (4.5-5.5), and in 0.1M solution of each of sodium sulfate, sodium nitrate, sodium perchlorate and potassium chloride as supporting electrolytes. The square-wave adsorptive cathodic stripping voltammogram of terazosin exhibited a single well-defined two-electron irreversible cathodic peak which may be attributed to the reduction of CO double bond of the drug molecule. A fully validated, simple, high sensitive, precise and inexpensive square-wave adsorptive cathodic stripping voltammetric procedure was described for determination of terazosin in bulk form, tablets and human serum. A mean recovery for 1x10(-8)M terazosin in bulk form, following preconcentration onto the hanging mercury drop electrode for 60s at a -1.0V (versus Ag/AgCl/KCl(s)), of 99+/-0.7% (n=5) was obtained. Limits of detection (LOD) and quantitation (LOQ) of 1.5x10(-11) and 5x10(-11)M bulk terazosin were achieved, respectively. The proposed procedure was successfully applied to determination of the drug in its Itrin((R)) tablets and human serum samples. The achieved LOD and LOQ of the drug in human serum samples were 5.3x10(-11) and 1.8x10(-10)M THD, respectively. The pharmacokinetic parameters of the drug in human plasma were estimated as: C(max)=77.5ngml(-1), t(max)=1.75h, AUC(0-t)=602.3nghml(-1), K(e)=0.088h(-1) and t(1/2)=11.32h) which are favorably compared with those reported in literature.

Polymeric matrix membrane sensors for sensitive potentiometric determination of some beta-blockers in pharmaceutical preparations.

Five poly(vinyl chloride) matrix membrane sensors responsive to some beta-blockers (atenolol, bisoprolol, metoprolol, propranolol and timolol) are described and characterized. The sensors are based on the use of the ion-association complexes of the beta-blocker cations with tungstophosphate anion as electroactive materials. The performance characteristics of these sensors, evaluated according to IUPAC recommendations, reveal fast, stable and near-Nernstian response for 10(-2)-2 x 10(-7) mol l(-1) of different beta-blockers over the pH range 2-9. Many inorganic and organic cations as well as drug excipients and diluents normally used in drug formulations do not interfere. The sensors are used for direct potentiometry of beta-blockers in some pharmaceutical preparations. Validation of the method according to the quality assurance standards shows suitability of the proposed sensors for use in the quality control assessment of these drugs. Results with an average recovery of 99.1% and a mean standard deviation of +/- 1.3% of the nominal are obtained which compare fairly well with data obtained using the British Pharmacopoeia method.

Ion-selective electrode for the determination of prenalterol.

A new prenalterol (Pr) ion-selective PVC membrane electrode based on the ion-pair complex of Pr with sodium tetraphenylborate was prepared and its performance characteristics were studied. The electrode exhibited a linear response with a good Nernstian slope over a relatively wide range of concentration. The electrode whose membrane was made of 8.0% (w/w) of ion pair, 49.5% (w/w) of dioctyl phthalate (DOP) and 43.5% (w/w) of PVC showed characteristics higher than those obtained with the other ones, namely, slope of 56.3 mV per concentration decade, at 25 degrees C; usable concentration range 1.2x10(-5)-3.2x10(-2) M prenalterol; response time

Polarographic determination of propranolol in pharmaceutical formulation.

Propranolol was reacted with nitric acid to give nitropropranolol and was then measured in Britton-Robinson solutions in the pH range 2.0-12.0 by differential-pulse polarography. Nitropropranolol gave rise to a well-resolved differential-pulse polarographic peak at pH 2.0. A linear calibration graph in the range 5.0 x 10(-7)-5.0 x 10(-5) M and a detection limit of 5 nM was obtained. The relative standard deviation was 1.95% (n = 10) at 5 x 10(-6) M. The effect of common exceipient on the peak height was evaluated. The method was applied for the determination of the drug in the tablet dosage form.

AAS and AES determination of furaltadone, methadone and trazodone in pharmaceutical formulations.

Ion-associate complexes of furaltadone, methadone and trazodone hydrochlorides with [Cd(SCN)(4)](2-) and [Zn(SCN)(4)](2-) were precipitated and the excess unreacted cadmium or zinc complex was determined. A new method using atomic emission and atomic absorption spectrometry for the determination of the above drugs in pure solutions and in pharmaceutical preparations is given. The drugs can be determined by the affort method in the ranges 7.2-72.16, 6.9-69.18 and 8.1-81.6 microg/ml solutions of the three drugs, respectively.

Indirect atomic absorption determination of atropine, diphenhydramine, tolazoline, and levamisole based on formation of ion-associates with potassium tetraiodometrcurate.

Ion-associate complexes of atropine sulphate (I), diphenhydramine HCl (II), tolazoline HCl (III) and levamisole HCl (IV) with potassium tetraiodomercurate were precipitated and their solubilities were studied as a function of pH, ionic strength and temperature. Saturated solutions of each ion-associate under the optimum precipitation conditions were prepared and the metal ion-content in the supernatant was determined. The solubility products were thus calculated at different temperatures. A new accurate and precise method using atomic absorption spectrometry for the determination of the investigated drugs in pure solutions and in pharmaceutical preparations is described. The drugs can be determined by the present method in the ranges 13.6--138.8, 5.6-58, 3.6--39.6 and 4.8--48 microg/ml solutions of I--IV, respectively.

AAS and spectrophotometric determination of propranolol HCl and metoprolol tartrate.

Two simple and accurate spectrophotometric methods are described for the determination of propranolol hydrochloride (I) and metoprolol tartrate (II). The methods are based on the reaction of each drug as a secondary amine: (a) with carbon disulphide, the formed complex extracted into iso-butyl methyl ketone (IBMK) after chelation with Cu(II) ions at pH 7.5, followed by measuring the absorbance at 435.4 nm or indirectly for the drug by flame atomic absorption spectrophotometry (AAS). The calibration graph is linear up to 40 and 60 microg ml(-1) with apparent molar absorptivities of 6.89 x 10(3) and 1.08 x 104 l mol(-1) cm(-1) and correlation coefficients of 0.9994 and 0.9995 for propranolol and metoprolol, respectively; (b) with pi-acceptors, tetracyanoethylene (TCNE), or chloranilic acid (CLA) to give highly coloured complex species. The coloured products are quantitated spectrophotometrically at 415 or 510 nm for the two drugs with TCNE and CLA, respectively, and obey Beer's Law with RSD less than 2.0. The methods were applied to the determination of these drugs in pharmaceutical preparation without interferences.