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The file attached to this record is the author's final peer reviewed version. The Publisher's final version can be found by following the DOI link. Anti-doping analysis requires an exceptional level of accuracy and precision given the stakes that are at play. Current methods rely on the application of chromatographic techniques linked with mass spectrometry to provide this. However, despite the effectiveness of these techniques in achieving good selectivity and specificity, some issues still exist. In order to reach the minimum required performance level as set by WADA, labs commonly use selective monitoring by quadrupole mass spectrometry. This can be potentially fooled through the use of masking agents or by moving the peaks, as often only a small portion of the spectrum is used for analysis. Further issues exist in the inability to detect new or modified compounds, or to reanalyse samples/spectra. One technique that could overcome these problems is that of comprehensive 2D chromatography. Here a second separation column is employed to generate greater separative power. Compared to conventional separation, GCxGC allows for a greater peak capacity (i.e., number of peaks that can be resolved within a given time) and greater separation of coeluting compounds, which makes the technique promising for the complex task required in anti-doping. When combined with Time of Flight Mass Spectrometry this technique demonstrates vast potential allowing for full mass range datasets to be obtained for retroactive analysis. Similarly, LCxLC provides improvements in resolving power compared to its 1D counterpart and can be used both online as part of the analysis or offline solely as a purification step. In this review we summarise the work in this field so far, how comprehensive chromatography has been applied to anti-doping studies, and discuss the future application for this technique.

This thesis is concerned with the preparation, and subsequent application of, hydrogels as devices for analysing axillary malodour in order to test the efficacy of antiperspirant / deodorant products. Using the well documented ability of hydrogels to absorb water and small molecules, the absorption, storage and subsequent extraction of a model sweat was investigated. Ten volatile fatty acids, one unsaturated aldehyde and one thiol were used in an aqueous solution to represent malodorous sweat in order to investigate the plausibility of such a device. \ud \ud Quantitative analysis of the malodorous compounds was carried out via GC-FID, with unknown compound identification carried out via GC-MS. Qualitative analysis was acquired with the addition of pH indicators such as bromophenol blue and quinine to the hydrogel device. \ud \ud The physical properties of the hydrogels were also probed by investigating a range of crosslinker concentrations and alternative hydrogel materials. The swelling kinetics in deionised water and the mechanical properties were investigated by dynamic mechanical analysis and Universal tester. \ud \ud Bacterial studies illustrated the hydrogels’ suitability for in vivo testing which then illustrated that the model protocol could be transferred to natural samples.\ud