Coffee is one of the most popular beverages that are widely consumed in the world. This study aimed to determine the caffeine in Nescafe, Cacao, Cappuccino, Coffee, using a UV-Visible spectrophotometer. In addition, studied caffeine stability in water. In the presented study, seventeen samples were collected from some Libyan markets. A simple, rapid, and, reliable extraction method for the determination of caffeine in the samples using dichloromethane, n-hexane, and methanol as the extracting solvents. The method is validated over a wide linear range of 2 – 10 µg/ml with correlation coefficients being consistently greater than 0.999. The minimum caffeine level was observed in the Nesquik (Cacao), Nestle Italian S.P.A sample (8.66 µg/ml), while the Nestle (Nescafe), Asbania sample showed the highest caffeine content (461.87ppm).The study of caffeine stability indicates that caffeine is stable in water for more than two weeks.