Pharmaceutical Analysis (Sheffield Analytical Chemistry)

This book concentrates on the analytical aspects of drug development and manufacture, focusing on the analysis of the active ingredient or drug substance. The book does not describe in detail the analysis of drug products – typically drug substances and excipients in a formulation. However, many of the approaches described for characterising drug substances can be applied to formulations, either by accounting for the presence of excipients in the analyte or by extracting and analysing the active ingredient.

The pharmaceutical industry is one of the most active areas for the application and development of new methods in the analytical sciences. This volume provides those joining the industry or other areas of pharmaceutical research with a source of reference to a broad range of techniques and their applications, allowing them to choose the most appropriate analytical technique for a particular purpose.

No book on the analysis of pharmaceutical materials should ignore the important area of quality and regulation. The first chapter provides an up-todate overview of the philosophy and practicalities of working in a regulated environment, with reference to current regulations and guidance.

Subsequent chapters cover the major disciplines of separation sciences and spectroscopy. Recognising the importance and breadth of the area of separation sciences, our authors concentrate on method development in high performance liquid chromatography (HPLC or LC), capillary electrophoresis (CE), gas chromatography (GC) and thin layer chromatography (TLC), discussing traditional approaches in addition to the newer computational and chemometric methods. One of the most important and challenging areas in the analysis of pharmaceuticals is the determination of chiral purity. It is therefore highly appropriate that a chapter is devoted to this area. The importance of chiral analysis is
described, together with the development of techniques across the separation sciences and beyond.

In considering the spectroscopies, the development and widespread use of coupled techniques forms a major part of the volume in the chapters covering nuclear magnetic resonance (NMR) and mass spectrometry (MS). In the NMR chapter, extensive coverage is given to state-of-the-art coupled LC/NMR. The chapter also covers multi-nuclear NMR, computer-aided spectral interpretation, quantitative NMR and solid-state NMR – all important techniques applied in the pharmaceutical development laboratory.

Recent years have seen many important developments in MS. This book devotes a chapter to the technique, focusing on the varied instrumental capabilities, their basic principles of operation and their applicability to pharmaceutical analysis. The applications of mass spectrometry, both in structure elucidation and quantitative analysis, are considered. Quantitative analysis MS is covered in detail, to allow the reader to gain background knowledge of a technique that is becoming important in drug substance analysis. Vibrational spectrosopy can be used to support structural elucidation by NMR and MS, but more typically it is used for identity testing, because IR and Raman spectra act as a fingerprint for molecular structure. However, both IR and Raman find their principal application in the investigation of polymorphism. Examples are described in this chapter, together with the benefits of coupling these techniques to microscopy.

Additional solid-state techniques are covered in the chapter on solid-state analysis and polymorphism. The determination and control of the solid-state form, in respect of both crystal structure and particle characteristics, are important. The physical properties of the drug substance will influence its behaviour during handling processes and formulation, and can have a dramatic effect on dissolution, solubility and therefore bioavailability. Although microscopy and imaging are used in a number of the above disciplines, a separate chapter is devoted to the use of optical and electron imaging techniques and image analysis, which play an increasingly important role in contaminant analysis and drug-excipient distribution.

The final chapter deals with the increasingly important area of process analytical science. There is increasing interest in in-process measurements from the FDA and other regulatory bodies, and this seems certain to be a rapidly expanding area of the analytical sciences in the pharmaceutical industry.

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