Articles and Columns

The purpose of this short review article is to highlight some capabilities of qNMR spectroscopic methods in drug quality evaluation, indicating that qNMR spectroscopy should be more often applied when chromatographic methods are not working effectively.

A number of analytical applications in the area of security screening, medical diagnosis, drug authentication and quality control often require non-invasive probing of diffusely scattering (turbid) media in order to obtain chemical characterisation of deep-lying sample regions. Examples include non-invasive disease diagnosis, the detection of concealed explosives and illicit materials, the identification of counterfeit drugs and quality control applications in the pharmaceutical industry. Raman spectroscopy holds particular promise in this area due to its inherently high chemical specificity [exceeding that of near infrared (NIR) absorption spectroscopy and comparable with mid-infrared and THz methods], the ability to probe samples in the presence of water (the Raman scattering cross-section of water is very low) and its high penetration depth into turbid non-absorbing or weakly absorbing samples. On the downside, the technique is restricted to samples that do not exhibit strong fluorescence emission although this problem can, in the majority of cases, be avoided by using NIR excitation. Until recently, Raman techniques have generally been confined to applications involving surface layers of turbid media due to limitations imposed by the backscattering collection geometry common to the majority of commercial Raman probes. In principle, confocal Raman microscopy can potentially resolve objects to depths of up to several hundred micrometres. Deeper layers cannot be readily resolved and, typically, are overwhelmed by Raman and fluorescence signals emanating from the surface layer.

UV/vis reflection spectroscopy is a practical method to investigate pulp ageing, especially when reflectance spectra are converted to absorbance (k/s) spectra. Even if detailed reaction paths cannot be solved with this technique alone, it provides a very fast and simple method to study the changes in the concentrations of certain important pulp components during ageing. In addition, the concentrations of these components have been studied also in other pulp processes, such as mechanical and chemical pulp bleaching.

Our focus here is analytical procedures and the role of nuclear magnetic resonance (NMR) in particular. These have, until now, largely relied on conventional chromatography, and vibrational spectroscopy—infrared (IR), Raman and near infrared (NIR) spectroscopy. In spite of inherent difficulties with peak assignment and reliable quantification, vibrational spectroscopy has been used to derive information on reaction progression to impart fundamental understanding. This article sets out a wider scope to show how NMR can play a key role. Furthermore, NMR integrates well with established procedures to provide a suite of useful technologies that make the PAT challenge tractable.

The last TD column showed the effect of calculating second derivatives on a set of 100 spectra, which will be the starting point for this column.

In the post-genome era, the focus of life science is shifting to proteins. Based on the difference between the various states of the protein, time resolved Fourier transform (tr-FT-IR) spectroscopy can selectively detect, with nanosecond resolution, reactions of the amino acids, the ligands and specific water molecules in the active centre of the protein, thereby providing a detailed understanding of the reaction mechanism. Malfunctioning of proteins is the cause of many diseases. Thus, the understanding of structure, function and interaction of proteins at the molecular level is essential for the development of drugs for a rational molecular therapy.

This article explains how BAS developed and maintained its pivotal position in the European iron and steel metrology community and explains in detail the important work done by its volunteers.

The University of Leicester began an investigation to determine whether useful information on PAN (Peroxyacetyl nitrate) could be obtained from MIPAS data using the MSF absorption cross-sections.

The authors show how the use of SIAM method (Species Identification of Animals MALDI-TOF mass spectrometry) is a fast and reliable tool for recognising the origin of mammalian species.