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This graduation thesis is about the development of a determination method for the tropane alkaloids, atropine and scopolamine and the analysis of various food categories for the presence of these compounds. Atropine and scopolamine are two of the most known tropane alkaloids. They originate from edible plants or from plants that are accidentally collected with the crops. They can be highly toxic to humans and deadly to infants and children. Analysis of atropine and scopolamine by LC-MS/MS is one of the methods recommended by EFSA for the monitoring of tropane alkaloids. However, a few detailed analytical procedures have been reported. The method combines great sensitivity and selectivity along with fast and accurate analysis. After experiments with different extraction solvents, such as acetonitrile instead of methanol and with or without the addition of formic acid, the following extraction solvent was used: CH3OH:H2O (3:2)+HCOOH 0.2%+ACN 0.2%. It showed good recovery results, efficiency and repeatability and great abundance of the peaks of atropine and scopolamine. Experiments with two different food samples, flour from the Italian market and imported noodles, were performed and the flour was chosen as the matrix for the preparation of the calibration curve. The calibration curves that were prepared with flour had very good linearity results, as R2 was both for atropine’s and scopolamine’s calibration curves equal to 0.9999. The samples that were checked for contamination belonged to seven different food categories: flour, pasta, tea/herbs, spices, cake, unknown samples and gallettes with rice. A total of sixty-two samples were analyzed. The contamination level was considered to be equal to 1ppb. Eighteen samples were found contaminated. Most of them were flour made from buckwheat of different Italian brands. The majority of the contaminated samples showed contamination of atropine and no contamination of scopolamine, while the samples that were contaminated with both alkaloids showed higher contamination in atropine than in scopolamine. The results can be explained by the ratio of these substances in the original plants from where these three samples were originated. A variety of other tropane alkaloids were found and identified in buckwheat, seeds (semi datura) and pulverized leaves (foglie datura) from the plant Datura stramonium. In the other food categories, a spice (fieno greco) was contaminated with scopolamine. Three out of ten unknown samples (one brand of baby food and two brands of flour) were contaminated with atropine and scopolamine.