Metabolomics is the study of small molecules (<1000 Da) present in a particular biological system. Since the metabolome is furthest downstream from the genome, it reflects activities at the functional level. Therefore it is of vital importance to develop robust and reliable analytical tools to study small molecules. Here, I describe the development of a metabolomics workflow using a home-built, electrokinetically driven, nano-spray sheath-flow interface to couple capillary zone electrophoresis (CZE) with electrospray ionization-mass spectrometry (ESI-MS). First, I will describe my work to develop rapid CZE-MS analyses of standard amino acids and a BSA digest. Then, I will detail my CZE-MS metabolomics workflow optimizations and applications with the C57BL6J mouse and Xenopus laevis model systems. Finally, I will describe the expansion of our CZE-MS capabilities by my work that allows operation of the CZE-MS interface with negative ion mode MS. Future work includes completion of an in-house metabolite library, system automation using a CZE auto-sampler, and incorporating metabolite quantitation into the workflow.