This paper discusses an analytical method namely solid phase extraction that is used to separate caffeine residue present in water samples. The developed method reported is in the aspect of sample extraction, mode operation, and selection of detector, figure of merit on method performance and analysis of real samples. Sorbents namely C18 and hydrophilic-lipophilic balance (HLB) have become the best selection for the intended purpose. Adjustments of pH, sample flow rate, sample volume, selection of suitable solvent (conditioning, eluting, and reconstituting sample), extraction time or retention time and other operating conditions for instruments are the main considerations during method developments of analytical works. Liquid or gas chromatography is widely used to detect analytes because it is highly selective and sensitive for trace analysis. The recovery assay determined is always high but it can be affected when extracted sample is introduced with the derivative agent prior to analysis. The concentration levels are commonly observed to be high in aquatic samples when the study area is linked to discharge activities, either directly or indirectly from a treatment plant. In cases of multi-residue analysis, caffeine is one of the high active pharmaceutical compounds reported and has become a dominant fraction of micro pollutants.