Supramolecular chemistry has expanded dramatically in recent years both in terms of potential applications and in its relevance to analogous biological systems. The formation and function of supramolecular complexes occur through a multiplicity of often difficult to differentiate noncovalent forces. The aim of this Review is to describe the crucial interaction mechanisms in context, and thus classify the entire subject. In most cases, organic host-guest complexes have been selected as examples, but biologically relevant problems are also considered. An understanding and quantification of intermolecular interactions is of importance both for the rational planning of new supramolecular systems, including intelligent materials, as well as for developing new biologically active agents.

Binding Mechanisms in Supramolecular Complexes

This review illustrates the need to use nuclear magnetic resonance (NMR) spectroscopy for the quantitative analysis of small molecules in their crude forms and in mixtures We provide the basic concepts of quantitative NMR (qNMR), a brief description of important acquisition and processing parameters responsible for obtaining high-quality, reproducible NMR spectra in order to maximize accuracy, and the latest referencing techniques used for quantitative analysis We also describe methods that are used for quantitative analysis including calibration-curve and standard-addition methods Further, we briefly address validation of qNMR spectroscopy and its major applications in various scientific disciplines

Quantitative 1H NMR spectroscopy

https://cyberleninka.org/article/n/398815.pdf

Analytical techniques in pharmaceutical analysis: A review

Based on a brief revision of what constitutes state-of-the-art “quantitative experimental conditions” for 1H quantitative NMR (qHNMR), this comprehensive review contains almost 200 references and covers the literature since 1982 with emphasis on natural products. It provides an overview of the background and applications of qHNMR in natural products research, new methods such as decoupling and hyphenation, and analytical potential and limitations, and compiles information on reference materials used for and studied by qHNMR. The dual status of natural products, being single chemical entities and valuable biologically active agents that need to be purified from complex matrixes, results in an increased analytical demand when testing their deviation from the singleton composition ideal. The outcome and versatility of reported applications lead to the conclusion that qHNMR is currently the principal analytical method to meet this demand. Considering both 1D and 2D 1H NMR experiments, qHNMR has proved to be h...

Quantitative 1H NMR: development and potential of a method for natural products analysis.

Recent analytical approaches in quality control of traditional Chinese medicines—A review

Quantitative NMR spectroscopy--applications in drug analysis.

NMR Spectroscopic and Molecular Modelling Studies on Cyclodextrin–Dipeptide Inclusion Complexes

The antibiotic agent gentamicin sulfate is a mixture of several structurally very similar aminoglycosides. The major components of gentamicin are gentamicin C1, C1a, C2 and C2a. These major components were separated by means of column chromatography. The 1H and 13C NMR spectra of the free bases and the corresponding sulfates were assigned using HMQC, HMBC and selective TOCSY experiments. Additionally, the 1H and 13C NMR spectra of the sulfates and hydrochlorides, respectively, of the minor components were assigned. The full assignment of all components of gentamicin is necessary for the quantitative analysis of batches of gentamicin. By means of coupled liquid chromatography–NMR, several different batches were studied, revealing different compositions of batches from various sources. Copyright © 2003 John Wiley & Sons, Ltd.

Assignment of the major and minor components of gentamicin for evaluation of batches

Micellar electrokinetic capillary chromatography, high performance liquid chromatography and nuclear magnetic resonance--three orthogonal methods for characterization of critical drugs.

High-resolution NMR spectroscopy is a powerful tool in the elucidation of a structure with respect to constitution, configuration and conformation. In recent years, NMR has been increasingly used in quantitative analysis. In this study, we show the ability of 1H NMR to determine the isomeric composition of the antidepressant drug fluvoxamine. The activity of fluvoxamine resides on the E-isomer, and the current British Pharmacopoeia limits the content of the Z-isomer to 0.5%. The NMR method described here is able to determine the content of the Z-isomer down to the 0.2% level on a total amount of 15 mg of the substance. Copyright © 2002 John Wiley & Sons, Ltd.

Ralph Deubner

Papers

Quantitative NMR spectroscopy--applications in drug analysis.

NMR Spectroscopic and Molecular Modelling Studies on Cyclodextrin–Dipeptide Inclusion Complexes

Assignment of the major and minor components of gentamicin for evaluation of batches

Micellar electrokinetic capillary chromatography, high performance liquid chromatography and nuclear magnetic resonance--three orthogonal methods for characterization of critical drugs.

Quantitative 1H NMR spectroscopic determination of the E/Z isomer ratio of the antidepressant drug fluvoxamine for use in pharmaceutical analysis