Spectrophotometric determination of fenoprofen calcium drug in pure and pharmaceutical preparations. Spectroscopic characterization of the charge transfer solid complexes.

Simple, accurate and robust spectrophotometric method was developed for determination of fenoprofen calcium drug (FPC). The proposed method was based on the charge transfer (CT) reaction of FPC drug (as n-electron donor) with 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), 2,4,6-trinitrophenol (picric acid, PA) or 1,2,5,8-tetrahydroxyanthraquinone (Quinalizarin, QZ) (as π-acceptors) to give highly colored charge transfer complexes. Different variables affecting the reaction such as reagent concentration, temperature and time have been carefully optimized to achieve the highest sensitivity. Beer's law was obeyed over the concentration ranges of 2-60, 0.6-90 and 4-30µgmL-1 using DDQ, PA and QZ CT reagents, respectively, with correlation coefficients of 0.9986, 0.9989 and 0.997 and detection limits of 1.78, 0.48 and 2.6µgmL-1 for the CT reagents in the same order. Elucidation of the chemical structure of the solid CT complexes formed via reaction between the drug under study and π-acceptors was done using elemental, thermal analyses, IR, 1H NMR and mass spectrometry. X-ray diffraction was used to estimate the crystallinity of the CT complexes. Their biological activities were screened against different bacterial and fungal organisms. The method was applied successfully with satisfactory results for the determination of FPC drug in fenoprofen capsules. The method was validated with respect to linearity, limit of detection and quantification, inter- and intra-days precision and accuracy. The proposed method gave comparable results with the official method.

A newly validated and characterized spectrophotometric method for determination of a three water pollutants metal ions.

A simple, fast and accurate spectrophotometric method had been developed to determine lead (II), chromium (III) and barium (II) ions in pure forms and in spiked water samples using thoron (THO) as a reagent forming colored complexes. It was found that the formed complexes absorbed maximally at 539, 540 and 538nm for Pb(II)-THO, Cr(III)-THO and Ba(II)-THO complexes, respectively. The optimum experimental conditions for these complexes had been studied carefully. Beer's law was obeyed in the range 1-35, 1-70, and 1-45µgmL-1 for Pb (II), Cr(III) and Ba(II) ions with THO reagent, respectively. Different parameters such as linearity, selectivity, recovery, limits of quantification and detection, precision and accuracy were also evaluated in order to validate the proposed method. The results showed that, THO was effective in simultaneous determination of Pb(II), Cr(III) and Ba(III) ions in pure forms and in spiked water samples. Also, the results of the proposed method were compared with that obtained from atomic absorption spectrometry. The isolated solid complexes had been characterized using elemental analysis, X-ray powder diffraction (XRD), IR, mass spectrometry and TD-DFT calculations. Their biological activities were investigated against different types of bacteria and fungi organisms.

In situ modified screen printed and carbon paste ion selective electrodes for potentiometric determination of naphazoline hydrochloride in its formulation.

The construction and performance characteristics of new sensitive and selective in situ modified screen printed (ISPE) and carbon paste (ICPE) electrodes for determination of naphazoline hydrochloride (NPZ-HCl) have been developed. The electrodes under investigation show potentiometric response for NPZ-HCl in the concentration range from 7.0×10-7 to 1.0×10-2 M at 25 °C and the electrode response is independent of pH in the range of 3.1-7.9. These sensors have slope values of 59.7±0.6 and 59.2±0.2 mV decade-1 with detection limit values of 5.6×10-7 and 5.9×10-7 M NPZ-HCl using ISPE and ICPE, respectively. These electrodes show fast response time of 4-7 s and 5-8 s and exhibits lifetimes of 28 and 30 days for ISPE and ICPE, respectively. Selectivity for NPZ-HCl with respect to a number of interfering materials was also investigated. It was found that there is no interference from the investigated inorganic cations, anions, sugars and other pharmaceutical excipients. The proposed sensors were applied for the determination of NPZ-HCl in pharmaceutical formulation using the direct potentiometric method. It showed a mean average recovery of 100.2% and 102.6% for ISPE and ICPE, respectively. The obtained results using the proposed sensors were in good agreement with those obtained using the official method. The proposed sensors show significantly high selectivity, response time, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ) compared with other proposed methods.

Potentiometric determination of ketotifen fumarate in pharmaceutical preparations and urine using carbon paste and PVC membrane selective electrodes.

This study compares between unmodified carbon paste (CPE; the paste has no ion pair) and polyvinyl chloride (PVC) membrane selective electrodes that were used in potentiometric determination of ketotifen fumarate (KTF), where sodium tetraphenylborate (NaTPB) was used as titrant. The performance characteristics of these sensors were evaluated according to IUPAC recommendations which reveal a fast, stable, and linear response for KTF over the concentration range of 10(-7) to 10(-2) mol L(-1). The electrodes show Nernstian slope value of 52.51 ± 0.20 and 51.51 ± 0.25 mV decade(-1) for CPE and PVC membrane electrodes at 30°C, respectively. The potential is nearly stable over the pH range 3.0-6.0 and 2.0-7.0 for CPE and PVC membrane electrodes, respectively. Selectivity coefficient values towards different inorganic cations, sugars, and amino acids reflect high selectivity of the prepared electrodes. The electrodes responses at different temperatures were also studied, and long operational lifetime of 12 and 5 weeks for CPE and PVC membrane electrodes, respectively, were found. These are used for determination of ketotifen fumarate using potentiometric titration, calibration, and standard addition methods in pure samples, its pharmaceutical preparations (Zaditen tablets), and biological fluid (urine). The direct potentiometric determination of KTF using the proposed sensors gave recoveries % of 98.97 ± 0.53 and 98.62 ± 0.74 with RSD 1.42 and 0.63% for CPE and PVC membrane selective electrodes, respectively. Validation of the method shows suitability of the proposed sensors for use in quality control assessment of KTF. The obtained results were in a good agreement with those obtained using the reported spectrophotometric method.

Potentiometric determination of antihistaminic diphenhydramine hydrochloride in pharmaceutical preparations and biological fluids using screen-printed electrode.

The performance characteristic of sensitive screen-printed (SPE) and carbon paste (CPE) electrodes was investigated for the determination of diphenhydramine hydrochloride (DPH) drug in pure, pharmaceutical preparations and biological fluids. Different experimental conditions namely types of materials used to prepare the working electrode (plasticizer), titrant, pH, temperature and life time were studied. Under these conditions, the SPE shows the best performance than CPE with respect to total potential change and potential break at the end point. The SPE and CPE exhibit suitable response to DPH in a concentration range of 1.0.10(-2) to 1.0.10(-6) mol/L with a limit of detection 9.70.10(-7) and 9.80.10(-7) mol/L, respectively. The slope of the system was 55.2±1.0 and 54.7±1.0 mV/decade over pH range 3.0-8.0 and 3-7 for SPE and CPE, respectively. Selectivity coefficients for DPH relative to a numbers of potential interfering substances were investigated. The SPE and CPE show a fast response time of 10 and 16s and were used over a period of 2 months with a good reproducibility. The sensors were applied successfully to determine DPH in pharmaceutical preparations and biological fluids. The results are compared with the official method.

Construction and performance characterization of screen printed and carbon paste ion selective electrodes for potentiometric determination of naphazoline hydrochloride in pharmaceutical preparations.

This paper describes the development of screen-printed (SPE) and carbon paste (CPE) sensors for the rapid and sensitive quantification of naphazoline hydrochloride (NPZ) in pharmaceutical formulations. This work compares the electroactivity of conventional carbon paste and screen-printed carbon paste electrodes towards potentiometric titration of NPZ. The repeatability and accuracy of measurements performed in the analysis of these pharmaceutical matrices using new screen printed sensors were evaluated. The influence of the electrode composition, conditioning time of the electrode and pH of the test solution, on the electrode performance were investigated. The drug electrode showed Nernstain responses in the concentration range from 1 × 10(-6) to 1 × 10(-2) mol L(-1) with slopes of 57.5 ± 1.3 and 55.9 ± 1.6 mV per decade for SPE and CPE, respectively, and was found to be very precise and usable within the pH range 3-8. These sensors exhibited a fast response time (about 3 s for both SPE and CPE, respectively), a low detection limit (3.5 × 10(-6) and 1.5 × 10(-6) M for SPE and CPE, respectively), a long lifetime (3 and 2 months for SPE and CPE, respectively) and good stability. The selectivity of the electrode toward a large number of inorganic cations, sugars and amino acids was tested. It was applied to potentiometric determination of NPZ in pure state and pharmaceutical preparation under batch conditions. The percentage recovery values for the assay of NPZ in tablets (relative standard deviations ≤0.3% for n = 4) were compared well with those obtained by the official method.