Coffee is one of the most popular stimulant beverages in the world, as it is highly rich source of an alkaloid component known as caffeine. On the other hand, people are using an ease and simplified preparation of coffee known as instant coffee, it also called soluble coffee, coffee crystals and coffee powder. This study aims to determine the level of caffeine in instant coffee samples randomly collected from Addis Ababa markets of Ethiopia by using UV-Vis spectrophotometer and high performance liquid chromatography (HPLC) techniques. Using these calibration curves the content of caffeine in the collected coffee samples; Nescafe, Abyssinia and Mac coffee determined in mg/g were 28.80 ± 1.91, 22.33± 0.21, and 13.20 ± 0.66 respectively, while using HPLC, caffeine content for those samples in mg/g were also 6.33 ±0.01, 3.99 ± 0.03, and 3.25 ± 0.12 in respective way. From the measured caffeine contents of each samples the content claimed by the manufacturer and the other research work reported were comparable with the analytical results obtained from HPLC method .From this work the amount of caffeine was also explained in dry weight analyzed using UV-Vis method was included in the range of 1.32 ± 0.07% - 3.92± 0.13%, and using HPLC was also in the range of 0.32± 0.012% - 0.63± 0.001%; this included in the range of the values of WHO and FAO stated. In general, the caffeine concentration (mg/g) in each coffee samples analyzed was in the order of Nescafe > Abyssinia coffee > Mac coffee using both UV-Vis and HPLC techniques.