New organic compounds that could serve as ligands for metals or in supramolecular assemblies were prepared by combining various amines and isothionates. This resulted in the new thiourea derivatives: 5,6-bis[aminoanilinomethanethione][1,10] phenanthroline (1), 1,2-bis[aminobenzo(15-crown-5)]-15-ylaminomethanethionebenzene (2), 5,6-bis[aminobenzo(15-crown-5)]-15-ylaminomethanethione[1,10]phenanthroline (3), and N-[1,10-phenanthroline]-N'- [[benzo-15-crown-5] yl]thiourea (4). The structures and compositions of the compounds have been confirmed by elemental analyses, UV-vis, FTIR, 1 H NMR (DMSO-d6), 13 C NMR (DMSO-d6) and MS spectra.
A novel, selective, sensitive and simple spectrophotometric method was developed and validated for the determination of the antidepressant duloxetine hydrochloride in pharmaceutical preparation. The method was based on the reaction of duloxetine hydrochloride with 1,2 naphthoquinone 4 sulphonate (NQS) in alkaline media to yield orange colored product. The formation of this complex was also confirmed by UV visible, FTIR, 1 H NMR, Mass spectra techniques and thermal analysis. This method was validated for various parameters according to ICH guidelines. Beer's law is obeyed in a range of 5.0-60 μg/mL at the maximum absorption wavelength of 480 nm. The detection limit is 0.99 μg/mL and the recovery rate is in a range of 98.10-99.57%. The proposed methods was validated and applied to the determination of duloxetine hydrochloride in pharmaceutical preparation. The results were statistically analyzed and compared to those of a reference UV spectrophotometric method.
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