Streamlined approach to high‐quality purification and identification of compound series using high‐resolution MS and NMR

Abstract

Automated medicinal chemistry (parallel chemistry) has become an integral part of the drug-discovery process in almost every large pharmaceutical company. Parallel array synthesis of individual organic compounds has been used extensively to generate diverse structural libraries to support different phases of the drug-discovery process, such as hit-to-lead, lead finding, or lead optimization. In order to guarantee effective project support, efficiency in the production of compound libraries has been maximized. As a consequence, also throughput in chromatographic purification and analysis has been adapted. As a recent trend, more laboratories are preparing smaller, yet more focused libraries with even increasing demands towards quality, i.e. optimal purity and unambiguous confirmation of identity. This paper presents an automated approach how to combine effective purification and structural conformation of a lead optimization library created by microwave-assisted organic synthesis. The results of complementary analytical techniques such as UHPLC-HRMS and NMR are not only regarded but even merged for fast and easy decision making, providing optimal quality of compound stock. In comparison with the previous procedures, throughput times are at least four times faster, while compound consumption could be decreased more than threefold.

Isolation and Identification of Flavones Responsible for the Antibacterial Activities of Tillandsia bergeri Extracts

“…Indeed, the combination of these two techniques allows a more efficient structural identification, the advantages of one overcoming the limitations of the other. 30 The aim of this study is to perform a phytochemical analysis and identify the antibacterial compounds present in T. bergeri. Bio-guided fractionation will be performed using agar overlay bioautography as a screening method against several Grampositive and Gram-negative bacterial strains as well as one resistant strain.…”

“…Following this, structural identification is performed using analytical techniques like nuclear magnetic resonance (NMR) and high-resolution mass spectrometry (HRMS). Indeed, the combination of these two techniques allows a more efficient structural identification, the advantages of one overcoming the limitations of the other …”

“…Indeed, the combination of these two techniques allows a more efficient structural identification, the advantages of one overcoming the limitations of the other. 30 …”