HPLC, TLC, and first-derivative spectrophotometry stability-indicating methods for the determination of tropisetron in the presence of its acid degradates

Three stability-indicating assay methods were developed for the determination of tropisetron in a pharmaceutical dosage form in the presence of its degradation products. The proposed techniques are HPLC, TLC, and first-derivative spectrophotometry (1D). Acid degradation was carried out, and the degradation products were separated by TLC and identified by IR, NMR, and MS techniques. The HPLC method was based on determination of tropisetron in the presence of its acid-induced degradation product on an RP Nucleosil C18 column using methanol-water-acetonitrile-trimethylamine (65 + 20 + 15 + 0.2, v/v/v/v) mobile phase and UV detection at 285 nm. The TLC method was based on the separation of tropisetron and its acid-induced degradation products, followed by densitometric measurement of the intact spot at 285 nm. The separation was carried out on silica gel 60 F254 aluminum sheets using methanol-glacial acetic acid (22 + 3, v/v) mobile phase. The 1D method was based on the measurement of first-derivative amplitudes of tropisetron in H2O at the zero-crossing point of its acid-induced degradation product at 271.9 nm. Linearity, accuracy, and precision were found to be acceptable over concentration ranges of 40-240 microg/mL, 1-10 microg/spot, and 6-36 micro/mL for the HPLC, TLC, and 1D methods, respectively. The suggested methods were successfully applied for the determination of the drug in bulk powder, laboratory-prepared mixtures, and a commercial sample.     

UV-sensitive indicators based on bromophenol blue and chloral hydrate dyed poly(vinyl butyral)

UV-sensitive indicators based on dyed poly(vinyl butyral) (PVB) containing acid-sensitive dye (bromophenol blue, BPB) and chloral hydrate have been developed and used successfully to measure the integrated UV irradiance. This flexible film changes colour from blue to green and finally to yellow on exposure to UV irradiation. The radiation-induced change in colour was analysed spectrophotometrically at the absorption band maxima of 421 and 601 nm. The film responds faithfully to UVA, UVB and UVC radiation, showing a maximum sensitivity at 200 nm. Correlations were established between the incident energy of UV radiation and the change in absorbance of BPB/PVB films at 421 and 601 nm using irradiation wavelengths of 248.5, 298.8 and 366 nm. The assessment of the uncertainties, the effect of the irradiation wavelength and chloral hydrate concentration on the performance of BPB/PVB films and the post-irradiation stability in different storage conditions were investigated.     

Morphological and macrostructural studies of dog cranial bone demineralized with different acids

Strong and weak acids were chosen for the bone decalcification process. Demineralization of dog cranial bone was carried out using 0.6 M concentration of either of hydrochloric, lactic or citric acid. Consequent morphologic changes were correlated with the developed chemistry, porosity and structure through XRD and FT-IR of the matrices. The dielectric permittivity, loss angle, relaxation dielectric loss as well as a.c. electrical conductivity as functions of frequency and temperature were measured. Zeta potential was evaluated at physiologic pH and temperature and correlated with the developed structures.The results prove lower dielectric properties of demineralized matrices compared to control and exhibited high dissipation of electric energy with more than one relaxation mechanism. This variation proves that the spectral behavior depended on the nature of the bone matrix which resulted from the phase compositions of bone and its crystallite size. The behavior of the obtained results is attributed to the differences of the demineralizing acids and their consequent actions on the matrices, i.e., the differences in the materials.     

Phytochemical,antimicrobial and antiquorum-sensing studies of pulicaria undulata L.: a revision on the structure of 1β,2α,3β,19α,23-pentahydroxy-urs-12-en-28-oic acid

Abstract

Phytochemical study of the aerial part of Pulicaria undulata L. led to the isolation of nine compounds. The structure of 1β,2α,3β,19α,23-pentahydroxy-urs-12-en-28-oic acid (4) was revised and confirmation of the stereochemical configuration of the hydroxyl groups was established using NOESY and selective decoupling experiments. The other compounds were identified as 1,2-dehydro-1,10α-dihydropseudoivalin (1), axillarin (2), grandifloric acid-15-β-glucoside (3), myrianthic acid (5), caffeic acid (6), quercetin (7), paniculoside IV (8) and caffeic anhydride (9). The structures were characterized by 1?D, 2?D NMR spectroscopy and confirmed with HRMS. Antimicrobial and antiquorum-sensing activities of the different extracts and isolated compounds of the plant were investigated. Generally, the phenolic rather than the terpenoidal compounds exhibited remarkable antimicrobial and antiquorum-sensing activity.

     

Action of 1,2-diamines and o-aminophenols on 1-alkyl-3-carboxyindole-2-acetic acid anhydrides. Preparation of new ring systems

1-Alkyl-3-carboxyindole-2-acetic acid anhydrides (I) react with ethylenediamine and with o-phenylenediamine to give directly 10-alkylimidazo[3,2:1′,2′]pyrido[4,5-b]indol-5(1H)-ones (II) and 5,6-dihydro-5-alkyl-13H-indolo[2′,3′:4,5]pyrido[1,2-a]benzimidazol-13-one (V), respectively. However, anhydrides I react with o-aminophenol and with o-aminothiophenol to give carboxyindole-acetanilide derivatives IX, which can be cyclised to indolo[2′,3′:4,5]pyrido[2,1-b]benzoxazolone and indolo[2′,3′:4,5]pyrido[2,1-b]benzthiazolone (XI). Some derivatives of II and V were prepared to help in elucidating the structures.     

A novel method for the synthesis of 1-aryltetrahydroisoquinolines

Carbenium ions generated from substituted benzhydryls using acid catalysis undergo smooth intramolecular trapping by pendant sulfonamide groups to provide excellent yields of 1-aryltetrahydroisoquinolines.     

N-sulfonylbenzotriazoles as advantageous reagents for C-sulfonylation

[Structure: see text]. Reactions of readily available N-(alkyl-, aryl-, and heteroarylsulfonyl)benzotriazoles 3a-h with diverse nitriles, reactive heteroaromatics, alkylheteroaromatics, sulfones, and esters produced alpha-cyanoalkyl sulfones 5a-i, sulfonylheteroaromatics 7a-e, alpha-(sulfonylalkyl)heterocycles 9a-f, alpha-sulfonylalkyl sulfones 11a-g, and esters of alpha-sulfonyl acids 14a-c, respectively, in synthetically useful to excellent yields. The results represent the first examples of the successful application of sulfonylazoles for C-sulfonylation.