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Highlights: [•] A qNMR method was used for direct assay determination of iobitridol in an injectable formulation. [•] Experiments were carried out in deuterated alkaline water with 3,5-dinitrobenzoic acid as internal reference standard. [•] Method was validated by assessing specificity, accuracy, precision, linearity, stability of samples and robustness. [•] Method proved suitable for routine controls especially when high sample throughput is required. [Copyright &y& Elsevier]

Falsification of drugs, entailing the use of drug substances from unknown unapproved suppliers, is one of the main concerns for the quality of medicines. Therefore, traceability of active ingredients represents an effective tool to fight the illegal trade of medicinal products. In this view, the present pilot study explores the profile of carvedilol active ingredients and possible differences related to the origin. Sixteen samples were examined by near-infrared spectroscopy (NIR), proton nuclear magnetic resonance ( 1 H-NMR spectrometry) and liquid chromatography mass spectrometry (LC-MS) Q-TOF and the data were analysed by principal component analysis (PCA), cluster analysis and PLSDA discriminant analysis. The results evidenced that the combined information from the three techniques gave good classification of the samples neatly distinguishing the APIs from European countries from the APIs manufactured out of Europe. In particular, NIR spectroscopy provided effective separation between European and non-European manufacturers and 1 H-NMR or LC-MS added specific information related to the separation. Concerning LC-MS Q-TOF, the analysis of multiple isobaric peaks proved to be highly predictive of the drug substance origin and emerged as a promising tool in the field of medicine traceability.

Substituted 4-heteroaryl-2-phenylquinolines were synthesized and tested on NK-2 and NK-3 receptors in order to get a better insight in the structure-activity relationship. On the whole, these molecules, which can be regarded as bioisosters of the NK-3 antagonist SB 218795, displayed a lower activity than the template. Ring electronic distribution and H-bond donor and acceptor positions played some role in selectivity, 2-imidazolyl substituted 2a showing affinity mainly towards NK-3 while 3-pyrazolyl substituted 4 displayed a preferential interaction with NK-2 receptor. Structural characterization of the synthesized compounds was achieved by NMR and mass techniques. Bidimensional 1H-NOESY experiments were a helpful tool for the assignment of the isomeric structures of compounds 9 and llb-c.