Spectrofluorimetric determination of guanethidine sulphate,guanfacine hydrochloride,guanoclor sulphate and guanoxan sulphate in tablets and biological fluids,using benzoin

A sensitive and rapid Spectrofluorimetric method for the determination of guanethidine sulphate, guanfacine hydrochloride, guanoclor sulphate and guanoxan sulphate in tablets and spiked human serum and urine samples is described. The method is based on the reaction of monosubstituted guanidino compounds in an aqueous potassium hydroxide solution with benzoin, in the presence of -mercaptoethanol and sodium sulphite. Highly fluorescent derivatives were obtained, with excitation and emission maximum wavelengths around 325 and 430 nm, respectively. In optimal reaction conditions, the linearity ranges were 0.04–0.28 g/ml, with relative standard deviations less than 2%. The method has been successfully applied to the determination of these drugs in tablets. The results are highly correlated with the B.P. method. Chloroform (or for guanoxan dichloromethane) was used to extract the drugs from serum and urine at basic pH, followed by the proposed fluorimetric method. The limit of detection is 0.02 g/ml for the selected drugs.     

Studies on the liquid-liquid extraction and ion and precipitate flotation of Co(II) with decanoic acid

The liquid-liquid extraction, ion and precipitate flotation of Co(II) from chloride media of 1·10^–4M initial Co(II) concentration and =0.1 have been investigated using decanoic acid and the results are compared. Organic solvents used were chloroform in the case of liquid-liquid extraction and ethanol (used as a solvent for the collector and a frother) in the case of flotation. From the results it appears that liquid-liquid extraction takes place through the formation of the complex: (CoR₂)₂(HR)₂ but flotation occurs through the formation of a surface active product which has the empirical formula CoR₂. The effects of pH and of decanoic acid concentration on the three separation processes were also investigated and the results discussed. Good agreement was observed between the experimental precipitate flotation curves and the theoretical curve calculated from the data published for Co(II) hydrolysis.     

Highly accurate vibration–rotation Franck–Condon factors for high levels

Highly accurate vibration–rotation Franck–Condon factors q^ab, for a transition between two diatomic electronic states (a) and (b), are sought. When the potentials of states (a) and (b) are of the RKR type, the computation of q^ab is reduced to that of Franck–Condon integral ?^ab(i) = ∫ ψ^a(r)ψ^b(r) dr in an interval r_i, r_i+1. By using convenient interpolations for the potentials U^a and U^b in the considered interval, this integral becomes ?^ab(i) = ∑ δ (r_i+1 – r_i)ⁿ⁺¹/(n + 1), where the “coupling constants” δ depend uniquely on the eigenvalues E^a and E^b of the considered transition and on the potentials U^a and U^b (the number N of terms depends on the desired accuracy). The method used computes the Franck–Condon factors q^ab without the explicit use of the wave function and by replacing the integrals by simple summations. To test the values of q^ab obtained by this method, the orthogonality rule ∫ ψ_v′ψ_v″ dr = 0 (for v′ ≠ v″) is used for one state or the other. This test, along with other tests, show that the Franck–Condon factors computed by the present method are accurate to nine significant figures for high and low levels.     

Synthesis of Important New Pyrrolo[3,4‐c]Pyrazoles and Pyrazolyl‐Pyrrolines from Heterocyclic β‐Ketonitriles

Treatment of heterocyclic β‐ketonitriles 1a,b with hydrazine hydrate and phenylhydrazine afforded the hydrazine derivatives 2a‐d which cyclized in PPA into pyrrolo[3,4‐c]pyrazoles 3a‐d. Reaction of 1a,b with cyanoacetohydrazide furnished the cyanoacetyl pyrrolo[3,4‐c]pyrazoles 4a,b. The hydrazine 2c reacted with β‐diketone and β‐ketoesters to afford pyrazolyl‐pyrrolines 5‐7. Also the later hydrazine reacted with some D‐aldoses and aceteophenone to give the corresponding hydrazones 10‐12 and hydrazine carboxamide derivatives 15a,b respectively.     

Separation of Co(II) from dilute aqueous solutions by precipitate and adsorbing colloid flotation

Ion, precipitate and adsorbing colloid flotation of cobalt(II) have been investigated at different pH values, using N-dodecylpyridinium chloride (DPCl), A strong cationic surfactant, and sodium lauryl sulfate (NaLS), a strong anionic surfactant, as collectors. In case of adsorbing colloid flotation, hydrous manganese dioxide was used as an adsorbent. The precipitate flotation curves experimentally obtained with the two tested collectors were compared with the corresponding theoretical one calculated from the data published for Co(II) hydrolysis. The effects of the collector concentration, ageing of the water-MnO₂–Co(II) system, bubbling time period, cobalt(II) concentration and foreign salts on the percent removal of Co(II) by adsorbing colloid flotation using DPCl as collector were determined. Removals approaching 100% could be achieved under the optimum conditions.     

REALISIS: a medicinal chemistry-oriented reagent selection, library design, and profiling platform

REALISIS is a software system for reagent selection, library design, and profiling, developed to fit the workflow of bench chemists and medicinal chemists. Designed to be portable, the software offers a comprehensive graphical user interface and rapid, integrated functionalities required for reagent retrieval and filtering, product enumeration, and library profiling. REALISIS is component-based, consisting of four main modules: reagent searching; reagent filtering; library enumeration; and library profiling. Each module allows the chemist to access specific functionalities and diverse filtering and profiling mechanisms. By implementing the entire process of reagent selection, library design, and profiling and by integrating all the necessary functionalities for this process, REALISIS cuts the time required to design combinatorial and noncombinatorial libraries from several days to a few hours.     

Optical absorption of tetraphenylporphyrin thin films in UV-vis-NIR region

The optical absorption of thermally evaporated tetraphenylporphyrin (TPP) in the UV-vis-NIR region have been studied. The absorption spectra recorded in the UV-vis region for the as deposited and annealed films showed different absorption bands, namely the Soret(B) at region 360-490nm, Q-band region consist of four bands in the region 500-720nm and two other bands labeled N and M in UV region. The Soret band always shows its characteristic effect splitting in all the TPP thin films and the effect of annealing on the intensities of these components have been observed. The spectra of the infrared absorption allow characterization of vibrational modes for the powder, as deposited and annealed thin films. Some of the optical absorption parameters, namely molar extinction coefficient, varepsilon, half band width, Deltalambda, electronic dipole strength, q(2) and oscillator strength, f, of the principle optical transitions have also been evaluated.     

Use of pi-acceptors for spectrophotometric determination of dicyclomine hydrochloride

Simple, rapid, accurate, and sensitive spectrophotometric methods are described for the determination of dicyclomine hydrochloride. The methods are based on the reaction of this drug as an n-electron donor with 2,3-dichloro-5,6-dicyano-p-benzoqunione (DDQ), p-chloranilic acid (p-CA), and chloranil (CL) as pi-acceptors to give highly colored complex species. The colored products are measured spectrophotometrically at 456, 530, and 650 nm for DDQ, p-CA, and CL, respectively. Optimization of the different experimental conditions were studied. Beer's law was obeyed in concentration ranges of 20-100, 50-250, and 80-600 microg/mL for DDQ, pCA, and CL, respectively. Colored complexes are produced in organic solvents and are stable for at least 1 h. The methods were applied to Spasmorest antispasmotic tablets and ampoules with good accuracy and precision.     

A facile synthesis of novel triazoloquinoxahnones and triazinoquinoxalinones

A series of 1-aryl-s-triazolo[4,3-a]quinoxalin-4-ones, 3 , were synthesized via the pyrolysis of the corresponding hydrazones, 6 . Thus, the cyclodehydrogenation occurred by refluxing them in an inert solvent (e.g. ethylene glycol) to give the triazoloquinoxalin-4-ones in a satisfactory yield. Using DMSO as a solvent for the above transformation afforded as a minor by-product an S-ylid. In contrast to earlier findings, annelation of a six-membered ring was successful and achieved through the pyrolysis of the pyruvate hydrazones derived of the quinoxalin-4-ones at ?230° to give the as-triazino[4,3-a]quinoxalin-5-ones, 4 . The reaction of 5 with acetylacetone afforded 3-(3′,5′-dimethylpyrazol-1-yl)-2(1H)-quinoxalinone, 10 . The structural assignments for the new compounds were based on their elemental analysis and spectroscopic data as well as an independent synthesis.