This work represents the development of novel methods of analysis for a wide range of metals, in particular germanium. This research has identified a range of foodstuffs and supplements containing low level concentrations o f germanium. In total germanium was quantified in 28 samples including vegetables such as beetroot (3 23/g)> garlic (2 78^ig/g) and potato (1 85|ng/g) and tablet formulations such as aloe vera tablet (20 83 jug/g), ginger tablet (9 96^g/g) and ginseng tablet (5 48|j.g/g). This work represents the first investigation for germanium content of a number of the samples. Ge-132 has been reported to have an antioxidant activity which has been linked to its medicinal properties. This work represents the first reported selective separation and identification of germanium dioxide and ge-132 in a range of food samples utilising mid-IR spectroscopy. The application o f a unique scoring system offers a rapid, non destructive and cost effective method of analysis. The first reported reverse phase HPLC methods for the determination of ge-132 was also developed. These methods at pH 3 and 4 are the first free from germanium dioxide interference and have wide linear ranges free from interference of metal ions such as Mg (II), Fe (II) and Zn (II). The investigation o f novel quercetin/metal complexation was completed. A novel method for the determination of Cr (III) was developed and this was applied to the quantification of Cr (III) in a commercial food supplement. This work also developed novel complexes of Pb (II) and Sb (III) with UV / Vis and fluorescent characterisation The LOD for Pb (II) achieved in the jig / L range is acceptable for application to sample analysis.