The development of a method for high throughput analysis of human finger and toe nail samples was required for the analysis of 4000 samples in association with the BRAVE (Bangladesh Risk of Acute Vascular Events) project. The aim of this project is to determine whether arsenic metabolites influence cardiovascular disease by comparing the metabolite concentrations in a control group and a group that have suffered stroke. The main objectives of this part of the project were to test for an extraction/digestion method that would allow for testing of total metals without destroying arsenic metabolites, to overcome the problem of small sample volume and to limit steps in sample preparation to reduce the risk of contamination. Method development was carried out on human nails of mixed ethnicity, which included digestion and buffer optimization and gave recoveries between 80-120% of both organo-arsenic metabolites. Areas of development that were identified after testing Bangladeshi nail samples were matrix problems which necessitate buffer optimization and a lack of homogeneity which may require different sample preparations procedures.