This study quantifies and compares the caffeine concentration (mg/L) of commercial espresso versus locally harvested Indigenous Yaupon Holly (Ilex vomitoria) in Pineville, Louisiana. The research evaluates how processing variables—specifically drying methodologies (air-dried, light roast, dark roast) and particle size (coarse vs. fine)—affect the final alkaloid yield. Using an aqueous extraction followed by liquid-liquid extraction (LLE) with dichloromethane (CH2Cl2), caffeine was isolated and quantified gravimetrically. Results indicate that while commercial espresso yielded the highest concentration (168\ mg/L), Yaupon Holly produced significant moderate yields, peaking in fine-ground, air-dried samples (98\ mg/L).