Major process related unknown impurity associated with the synthesis of Hydralazine hydrochloride bulk drug was detected by high performance liquid chromatography (HPLC) and was subjected to high resolution accurate liquid chromatography mass spectroscopy (HR/AM-LCMS) for identification. The proposed impurity was isolated from Hydralazine hydrochloride active pharmaceutical ingredient (API) by preparative chromatographic method and was injected on HPLC for comparison of retention time with that of the unknown process related impurity in Hydralazine hydrochloride. The molecular ion peak of preparatively isolated impurity and that of unknown process related impurity in Hydralazine hydrochloride were compared for confirmation. The postulated structure was unambiguously confirmed with the help of HR/AM-LC MS/MS, NMR and FTIR data proposed to be 1-(2-phthalazin-1-ylhydrazino)phthalazine (Hazh Dimer). This impurity of
Several new complexes of some transition metal ions with organometallic compounds were derived from ferrocencecarboxylaldehyde and 4-amino-2-hydroxy pyridine. These organometallic complexes were investigated by using some analytical techniques like infrared, mass spectra, electronic spectra, electron spin resonance, thermal analysis, magnetic moment, conductivity and antimicrobial activity. From the obtained elemental analysis data, organometallic compounds complexes shows 1:2 [M: L] ratio and general formula of the complex is [ML 2 .2H 2 O]. These complexes revealed a non-electrolytic nature. The magnetic moment values of the complexes exhibited the paramagnetic as well as diamagnetic in nature. The coordination behavior of the metal ions towards to the investigated organometallic compounds takes place through >C=N-and-OH groups. The electronic spectral data shows that all the complexes are covalent in nature, octahedral structure with coordination number six. Organometallic compound complexes were loses two water molecules subjected to simultaneous thermo gravimetric analysis, to study their decomposition mechanism and thermal stability. Mass spectra of the organometallic compound and their complexes are matched with theoretical values of the masses. The prepared organometallic compounds and their metal complexes were screened for their antibacterial activity against some bacterial species, Escherichia coli, Pseudomonas aeruginosa and Staphylococcus Pyogones. The Antimicrobial activity data show the metal complexes to be more active than the parent organometallic compounds.
The synthesis, characterisation, spectral studies, antibacterial and fugal studies of some transition metal ions like Mn ++ , Co ++ , Ni ++ , Cu ++ , Pd ++ and Pt ++ complexes of ferrocene based Organometallic compounds have been reported. The coordinate bonding of nitrogen to the central metal atom which reduces the electron density in the both azomethine link and thus lower the-HC=Nabsorption. The elemental analysis data exhibit the formation of 1:1 [M: L] ratio with coordination number six in the all complexes. The complexes have with octahedral geometry and D 4 h symmetry. The ferrocene based organometallic compound shows a molecular ion peak at m/z 482.4 which is equal to theoretical molecular weight. The molar conductance value indicates that, they are non-electrolytic in nature. These complexes were tested with some bacteria and fungi.
The aim of this research work is to develop a suitable HPLC method for the quantitative determination of process impurity (4-Bromophenyl) {Pyridine-2-yl} Acetonitrile as this compound is organic cyano compound hence it is necessary to quantify at ppm level presence of Brompheniramine Maleate Active Pharmaceutical Ingredient. Hence the HPLC method was developed on Instrument Waters 717 plus Auto Sampler, Waters 2487 Dual _ Absorbance Detector, Waters 2695 Separation Module, Waters 996 PDA Detector with Empower 2 Software on HPLC column Varian C18, 150 x 4.6 mm, 5μ at a flow rate of 1.5 mL/min. The limit of detection and the limit of quantitation for the impurity were established. Validation of the new developed HPLC method was carried out as per requirements of ICH guideline and the data shows that the proposed method is specific, linear, accurate, precise and robust. This method has been tested in a number of Brompheniramine Maleate samples and used successfully for quantification of the impurity at ppm level. The developed HPLC method was found to be suitable to quantify this impurity (4-Bromophenyl) {Pyridine-2-yl} Acetonitrile at ppm level present Brompheniramine Maleate.
scite is a Brooklyn-based organization that helps researchers better discover and understand research articles through Smart Citations–citations that display the context of the citation and describe whether the article provides supporting or contrasting evidence. scite is used by students and researchers from around the world and is funded in part by the National Science Foundation and the National Institute on Drug Abuse of the National Institutes of Health.