PubMed · 5907957
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M Trnková. 1966. [Adipiodon].. https://pubmed.ncbi.nlm.nih.gov/5907957/
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The adaptation of diverse organic reactions to solid supports requires significant reaction optimization efforts. A convenient on-support analytical method functionally similar to TLC in solution chemistry is very advantageous. As a TLC-equivalent method, the single bead FTIR is a simple, sensitive, fast, and convenient analytical method to monitor SPOS without stopping the reaction or cleaving the product. As with TLC, single bead FTIR provides a wide range of information such as qualitative assessment, quantitative determination, and reaction kinetics. Studies with the single bead FTIR have not only provided a tool for daily monitoring of the solid-phase reactions, but a way to understand the properties of polymer-bound substrate and the nature of polymer-supported organic reactions. It has assisted in the selection of a wide range of reaction conditions rapidly for SPOS in the rehearsal phase of combinatorial chemistry. Due to its convenience and efficiency, FTIR internal reflection spectroscopy has evolved as a useful analytical methodology for monitoring of combinatorial chemistry reactions directly on polymer surface.
In the past few years, the emergence of combinatorial chemistry has drawn increasing attention and a great deal of analytical research has been centered around this new methodology. These new methods capable of producing vast numbers of samples, which are in many cases highly complex, demand fast and reliable analytical techniques able to provide high quality information concerning sample compositions. Mass spectrometry (MS) is the method of choice to face these analytical challenges. In particular, the introduction of electrospray ionization (ESI and matrix assisted laser desorption/ionization (MALDI) have been the driving forces for many of the recent innovations, not only within the fields of the biosciences, but also in combinatorial chemistry. These ionization techniques are extremely versatile for the characterization of both single compound collections and compound mixture collections. The high-throughput capabilities, as well as many possible couplings with separation techniques (HPLC, CE) have been thus facilitated. However, mass spectrometry is not only limited to use as an instrument for synthesis control, but also plays an increasing role in the identification of active compounds from complex libraries. Recently, new initiatives for library analysis and screening have arisen from the application of the latest developments in mass spectrometry, Fourier transform ion cyclotron resonance (FTICR).
The advent of combinatorial and parallel synthesis methodologies in drug discovery have necessitated the development of analytical techniques which permit high throughput quantitative analysis of mixtures of small organic molecules. High pressure liquid chromatography with evaporative light scattering detection has become the major tool for this task. In this article we briefly review the theory of evaporative light scattering detection and the design of commercial instruments, as well as discuss the operational constraints imposed by the exigency of analyzing en masse the product libraries generated by these new drug discovery methods. The application of evaporative light scattering detection to library analysis is illustrated using examples from our library synthesis program. Complemented by ultraviolet absorbance detection for purity assessment and mass spectrometry for product identification, evaporative light scattering detection is the only technique affording sufficient accuracy and sensitivity for high throughput library analysis.