Determination of nicotinamide by stopped-flow injection method in pharmaceutical formulations

A simple stopped-flow injection system with spectrophotometric detection was proposed for the determination of nicotinamide (NAM) in pharmaceutical formulations. In this system cyanogen chloride formed from the combination of an acidic KSCN with the NaClO streams reacts with injected NAM to form glutaconic aldehyde. Then the product of these three components was coupled with another buffered (pH 3.5) stream of barbituric acid and directed towards the detector. A 45 s after sample injection the pump was stopped for 130 s. During this time the reactants in the flow cell were provided with the required temperature (40 °C) by placing the cell in a home made cell jacket to increase the yield of the polymethine dye product. Eventually, the absorbance of the formed pink color dye was monitored spectrophotometrically at 560 nm and NAM in the concentration range of 1.0–25.0 μg/mL (R = 0.9974 and D.L = 0.5 μg/mL) was determined. The results obtained by this method were compared statistically and agree with those obtained by the method described in the British Pharmacopoeia.     

Optical metal-organic framework sensor for selective discrimination of some toxic metal ions in water

This paper reports the development of a facile and effective approach, based on the use of Zr-based metal-organic frameworks (UiO-66) sensor with micropores geometry, shape and particle morphology for the visual detection and removal of ultra-traces of some toxic metal ions such as Bi(III), Zn(II), Pb(II), Hg(II) and Cd(II). UiO-66 was used as selective carriers for accommodating hydrophobic chromophore probes such as dithizone (DZ) without coupling agent for sensitive and selective discrimination of trace level of toxic analytes. The developed UiO-66 sensor was utilized for the detection of ultra-traces of some toxic metal ions with the naked eye. The new sensor displays high sensitivity and selectivity of a wide range of detectable metals analytes up to 10⁻¹⁰ mol dm⁻³ in solution, in a rapid analyte uptake response (seconds). The developed sensor is stable, cost effective, easy to prepare, and would be useful for rapid detection and removal of ultra-traces of toxic metal ions in water samples.     

Comparison of HPLC and MEEKC for Miconazole Nitrate Determination in Pharmaceutical Formulation

A simple solid phase extraction (SPE) method coupled with high performance liquid chromatography (HPLC) using UV detector and microemulsion electrokinetic chromatography (MEEKC) has been developed and compared for the quantitative determination of miconazole nitrate in pharmaceutical formulation. For HPLC method, two parameters were optimized, namely, the wavelength and the mobile phases. The optimized condition was at the 225 nm wavelength and the mobile phase of ACN:MeOH (90:10 v/v). There are seven MEEKC parameters that were optimized, in this research, which were applied to voltage, temperature, wavelength, sodium dodecyl sulfate (SDS) concentration, buffer pH, buffer concentration and butan-1-ol concentration. The optimum MEEKC condition was obtained using 86.35 % (w/w) 2.5 mM borate buffer pH 9, 0.25 % (w/w) SDS, 0.8 % (w/w) ethyl acetate, 6.6 % w/w butan-1-ol and 6.0 % (w/w) acetonitrile. The combination of SPE using a diol column with HPLC–UV and the MEEKC methods were successfully applied for the determination of miconazole nitrate in a pharmaceutical formulation with the recovery percentage of 98.35 and 92.50 %, respectively.     

Synthesis of a New Heteropolytopic Cryptand Through Schiff Base Condensation in the Presence of Ba(II) Ion

A new Schiff base cryptand (L) has been prepared via [2 + 2] condensation of 1,3,5-tris(2-formylphenoxymethyl)benzene (1) with 1,3,5-tris(aminomethyl)benzene trishydrochloride (2) in the presence of Ba(II) ion. The analytical data show that the Ba(II) cation is not retained by the product. Thus it seems that the role of the Ba(II) ion is to organize the transition state preceding the formation of the cryptand.     

Trichloromelamine (TCM) – Catalyzed Efficient and Selective Thioacetalization of Aldehydes and Transthioacetalization of Acetals and Oxathioacetals under Mild Reaction Conditions

Trichloromelamine was used effectively as a catalyst for thioacetalization of aldehydes and transthioacetalization of acetals and oxathioacetals under mild and almost neutral reaction conditions. By this method, aldehydes, acetals, and oxathioacetals were selectively protected in the presence of ketones as their 1,3-dithiolanes or 1,3-dithianes.     

Bulk polymer nanoparticles containing a tetrakis(3-hydroxyphenyl)porphyrin for fast and highly selective separation of mercury ions

We report on the synthesis of polymeric nanoparticles (PNPs) containing a tetrakis(3-hydroxyphenyl)porphyrin, and their use for the separation of mercury(II) ion. The PNPs were prepared by bulk polymerization from methacrylic acid (the monomer), ethyleneglycol dimethacrylate (the cross-linker), 2,2′-azobisisobutyronitrile (the radical initiator) and the mercury(II) complex of 5,10,15,20-tetrakis(3-hydroxyphenyl)-porphyrin. The Hg(II) ion was then removed by treatment with dilute hydrochloric acid. The PNPs were characterized by colorimetry, FT-IR spectroscopy, and scanning electron microscopy. The material is capable of binding Hg(II) from analyte samples. Bound Hg(II) ions can be eluted with dilute nitric acid and then quantified by cold vapor AAS. The extraction efficiency, the effects of pH, preconcentration and leaching times, sample volume, and of the nature, concentration and volume of eluent were investigated. The maximum adsorption capacity of the PNPs is 249 mg g^?1, the relative standard deviation of the AAS assay is 2.2 %, and the limit of detection (3σ) is 8 ng.L^?1. The nanoparticles exhibit excellent selectivity for Hg(II) ion over other metal ions and were successfully applied to the selective extraction and determination of Hg(II) ion in spiked water samples.

Quantum dynamics of heavy light heavy reactions: Application to (F + CH4 → FCH3 + H) reaction

We apply the time-dependent theory to the collinear exchange reaction F + CH₄ → FCH₃ + H. We have performed detailed calculations on two-dimensional potential surfaces representing the ground electronic potentials of the collinear F + CH₄ → FCH₃ + H reaction, at incident energies. Transmission coefficients range from zero to unity, depending upon the incident energy. Normal modes of vibrations are displayed along the reaction path.     

Highly Efficient Synthesis of 3,5-Diaryl-1,2,4-thiadiazoles in Water–Wet Paste Conditions

1,3-Dibromo-5,5-diphenylimidazolidine-2,4-dione (N,N’-dibromo phenytoin) was efficiently used for the rapid conversion of thiobenzamides to the corresponding 3,5-diaryl-1,2,4-thiadiazoles in water–wet paste conditions.

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Facile Synthesis of Benzotriazole Derivatives Using Nanoparticles of Organosilane-Based Nitrite Ionic Liquid Immobilized on Silica and Two Room-Temperature Nitrite Ionic Liquids

Nanoparticles of organosilane-based nitrite ionic liquid immobilized on silica, 1-butyl-3-methylimidazolium nitrite, and 1-(3-trimethoxysilylpropyl)-3-methylimidazolium nitrite were used as effective reagents for the preparation of benzotriazole derivatives from 1,2-diaminobenzenes at room temperature under mild solvent-free conditions. These ionic liquids play as nitrosonium sources in this procedure.1,2-Diaminobenzene derivatives have been treated with ionic liquids to give the related diaminobenzenes in very good to excellent yields in short reaction times.

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