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Over the past decade, the risk assessment of carcinogenic and genotoxic compounds in food has received increasing attention due to their capability of producing cancer by altering the genetic material of target cells directly in humans. Compounds that are both carcinogenic and genotoxic often presented at low levels in food, therefore, it is strenuous for regulators and food companies to evaluate the potential risk of these compounds in food. Alkenylbenzenes are a group of compounds, mostly present in edible consumer products such as essential oils, herbal medicines, plant foods, spices, and flavourings. Since 2001, the European Scientific Committee on Food considered that estragole, methyleugenol and safrole are genotoxic and carcinogenic. Eugenol and myristicin are weak hepatocarcinogenic, however, they are believed to be toxic in high dose. The development of analytical methods for food matrices has always been problematic due to the wide range of physicochemical features that might affect analyte structure and extraction efficiency as a result of varied processing during preparation and distribution. However, there have been many efforts being made to analyse and study thoroughly the impact of these alkenylbenzenes in consumable industry. Until now, there have been multiple proposed analytical techniques which are ranging from liquid chromatography, gas chromatography to capillary electrokinetic chromatography. In this thesis, the first part is a review of the 10-year period consisting of attainments in developing analytical techniques for the analysis of alkenylbenzenes starting from 2010. The second part of this study is to develop analytical methods (including sample preparation by solvent extraction) based on liquid chromatography and micellar electrokinetic chromatography to determine alkenylbenzenes in food samples. The alkenylbenzenes compounds of interest in this study are eugenol, methyleugenol, myristicin, safrole and estragole. Lastly, a solid-phase extraction using melamine sponge functionalised with Silica-C18 is established aiming to enhance sensitivity and extraction efficiency for the determination of alkenylbenzenes in food samples.