M.Tech. / Fungi and their mycotoxins are major contaminants of cereals and maize which is the major staple food for Angolan population. The consumption of fungal and mycotoxins contaminated maize can induce health problems as these mycotoxins are known to induce immune suppression and other chronic diseases known as mycotoxicoses. In addition, to these mycotoxins also induce chronic diseases such as cancers of various types (liver, oesophageal, brain). Mycotoxins also immensely affect organs such as fragility and haemorrhage in tissues, liver-necrosis, bile-duct proliferation, caustic effects, intestinal haemorrhage and diarrhoea, adenomatosis, tremors, inco-ordination, mania, coma, photosensitization, sloughing of the extremities, nephrosis, uremia, infertility, prolonged oestrus, huge implications and infections in people with Human immunodeficiency virus (HIV)- AIDS. There is a very little known about the incidence of mycotoxins in Angola, which are associated with Food, Environment and Health. Therefore, the aim of this scientific novel study in history of Angola was to analyse maize samples obtained from major markets in Angola and to establish their quality with regard to mycotoxins and fungi and well as to establish possible links to the prevalent diseases as well as chronic diseases recorded among Angolan populations. To attain these aims, 60 samples of maize were randomly selected and purchased from open rural and nonregulated informal (dusty and food exposed to open air) markets around Luanda, Angola. Luanda, being the capital city of Angola was found to be the best place to sample, because of the presence of huge markets in which food products as well as maize produced in different provinces are delivered and sold to its high population. Thus, sampling in these markets was representative of the whole country and the results obtained give an approximate the status of the quality of maize consumed in different parts of Angola. The result from this study approximates the status of possible health risks that consumers can be exposed due to consumption of these mycotoxins. The samples were analysed in the Food Environmental and Health Research Laboratories at the University of Johannesburg for fungi and mycotoxins contamination using fungal screening methodologies. In terms of mycotoxins extraction, a multi-mycotoxin (solvent-solvent) extraction, solid phase extraction using SAX column for fumonisins (FBs) and immuno-affinity column (VICAM) were used for confirmation of results. Normal thin layer chromatography (TLC), reversed phase thin layer chromatography (RPTLC) (both for FBs confirmation), fluorometer “VICAM” and high performance liquid chromatography (HPLC) were techniques used for mycotoxins detection, identification and quantification. From the results obtained in this study, fungal isolation revealed contamination of the three most important toxigenic species: Aspergillus, Penicillium, Fusarium spp.