Nuclear magnetic resonance spectroscopic analysis

Parrot, I., Huang, P.C., Khosla, C. 2002. Circular dichroism and nuclear magnetic resonance spectroscopic analysis of immunogenic gluten peptides and their analogs. J Biol Chem 277 455—412. 

Nuclear Magnetic Resonance Spectroscopic Analysis of Intact Kidney Tissue... 

Jarosszewski JW, Matzen L, Frolund B, Krogsgaard P. Neuroactive polyamine wasp toxins nuclear magnetic resonance spectroscopic analysis of the protolytic properties of philanthotoxin-343. J Med Chem 1996 39 515 521. 

Sherriff, B. L., Tisdale, M. A., Sayer, B. G., Schwarcz, H. P. and Knyf, M. (1995) Nuclear magnetic resonance spectroscopic and isotopic analysis of carbonized residues from subartic Canadian prehistoric pottery. Archaeometry 37, 95 111. 

Hutchinson, C.R. The use of isotopic hydrogen and nuclear magnetic resonance spectroscopic techniques for the analysis of biosynthetic pathways. J. Nat. Prod. 1982, 45, 27-37. 

Beckwith-Hall, B.M. Nicholson, J.K. Nicholls, A. Foxall, P.J.D. Lindon, J.C. Connor, S.C. Abdi, M. Connelly, J. Holmes, E. Nuclear Magnetic Resonance Spectroscopic and Principal Components Analysis Investigations into... 

Beckwith-Hall B M, Nicholson J K, Nicholls A W, et al. (1998). Nuclear magnetic resonance spectroscopic and principal components analysis investigations into biochemical effects of three model hepatotoxins. Chem. Res. Toxicol. 11 260-272. 

Infrared and nuclear magnetic resonance spectroscopic methods are applicable for analysis of soluble phenohc ptepolymers and solid products. 

Pullen, F. S., Swanson, A. G., Newman, M. J. and Richards, D. S., On-line liquid chromatography/nuclear magnetic resonance spectrometry — a powerful spectroscopic tool for the analysis of mixtures of pharmaceutical interest, Rapid Comm. Mass. Spectr., 9, 1003, 1995. 

Perhaps the most revolutionary development has been the application of on-line mass spectroscopic detection for compositional analysis. Polymer composition can be inferred from column retention time or from viscometric and other indirect detection methods, but mass spectroscopy has reduced much of the ambiguity associated with that process. Quantitation of end groups and of co-polymer composition can now be accomplished directly through mass spectroscopy. Mass spectroscopy is particularly well suited as an on-line GPC technique, since common GPC solvents interfere with other on-line detectors, including UV-VIS absorbance, nuclear magnetic resonance and infrared spectroscopic detectors. By contrast, common GPC solvents are readily adaptable to mass spectroscopic interfaces. No detection technique offers a combination of universality of analyte detection, specificity of information, and ease of use comparable to that of mass spectroscopy. 

As active substances are separated and purified they are characterized by a combination of spectroscopic analyses and chemical correlations. Particularly useful spectroscopic analysis techniques are nuclear magnetic resonance (proton and carbon), mass spectrometry and Infra-red and ultraviolet spectrophotometry. 

Spectroscopic analyses are widely used to identify the components of copolymers. Infrared (IR) spectroscopy is often sufficient to identify the comonomers present and their general concentration. Nuclear magnetic resonance (NMR) spectrometry is a much more sensitive tool for analysis of copolymers that can be used to accurately quantify copolymer compositions and provide some information regarding monomer placement. 

Modern spectroscopy plays an important role in pharmaceutical analysis. Historically, spectroscopic techniques such as infrared (IR), nuclear magnetic resonance (NMR), and mass spectrometry (MS) were used primarily for characterization of drug substances and structure elucidation of synthetic impurities and degradation products. Because of the limitation in specificity (spectral and chemical interference) and sensitivity, spectroscopy alone has assumed a much less important role than chromatographic techniques in quantitative analytical applications. However, spectroscopy offers the significant advantages of simple sample preparation and expeditious operation. 

Colquhoun, I.J. and Goodfellow, B.J. 1994. Nuclear magnetic resonance spectroscopy. In Spectroscopic Techniques for Food Analysis (R.H. Wilson, ed.), pp. 87-145. VCH Publishers, New York. 

Aside from the direct techniques of X-ray or electron diffraction, the major possible routes to knowledge of three-dimensional protein structure are prediction from the amino acid sequence and analysis of spectroscopic measurements such as circular dichroism, laser Raman spectroscopy, and nuclear magnetic resonance. With the large data base now available of known three-dimensional protein structures, all of these approaches are making considerable progress, and it seems possible that within a few years some combination of noncrystallo-graphic techniques may be capable of correctly determining new protein structures. Because the problem is inherently quite difficult, it will undoubtedly be essential to make the best possible use of all hints available from the known structures. 

These semisynthetic proteins have served as useful tools to investigate and study the role of Ras proteins in the cell, for instance, new insights in the so-called Ras acylation cycle could be obtained as well as solid-state nuclear magnetic resonance (NMR) spectroscopic analysis of the lipidated membrane anchor and proteins became possible. ... 

Infrared (IR) spectroscopy was the first modern spectroscopic method which became available to chemists for use in the identification of the structure of organic compounds. Not only is IR spectroscopy useful in determining which functional groups are present in a molecule, but also with more careful analysis of the spectrum, additional structural details can be obtained. For example, it is possible to determine whether an alkene is cis or trans. With the advent of nuclear magnetic resonance (NMR) spectroscopy, IR spectroscopy became used to a lesser extent in structural identification. This is because NMR spectra typically are more easily interpreted than are IR spectra. However, there was a renewed interest in IR spectroscopy in the late 1970s for the identification of highly unstable molecules. Concurrent with this renewed interest were advances in computational chemistry which allowed, for the first time, the actual computation of IR spectra of a molecular system with reasonable accuracy. This chapter describes how the confluence of a new experimental technique with that of improved computational methods led to a major advance in the structural identification of highly unstable molecules and reactive intermediates. 

The hyphenation of capillary electromigration techniques to spectroscopic techniques which, besides the identification, allow the elucidation of the chemical structure of the separated analytes, such as mass spectrometry (MS) and nuclear magnetic resonance spectroscopy (NMR) has been widely pursued in recent years. Such approaches, combining the separation efficiency of capillary electromigration techniques and the information-rich detection capability of either MS or NMR, are emerging as essential diagnostic tools for the analysis of both low molecular weight and macromolecular compounds. 

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