This study investigates the impact of distillation temperature on phenol content in coconut shell liquid smoke, a product derived from pyrolysis and subsequent condensation processes. Liquid smoke, renowned for its versatile applications including preservation, antioxidation, antiseptic, and antibacterial properties, necessitates distillation for both quality enhancement and safety. The research comprises a two-stage distillation, featuring 11 temperature variations (100-150°C) in the first stage and 9 variations (75-155°C) in the second stage. Characterization involves pH assessment and Gas Chromatography-Mass Spectrometry (GC-MS) analysis to identify chemical components. The pH range in the initial distillation stage spans 1.18-1.30, and the second stage ranges from 1.11-1.39. GC-MS analysis of raw coconut shell liquid smoke reveals 25 components, including phenol, furan, ketone, acid, alcohol, benzenediol and derivatives, alkyl aryl ether, deoxycytidine, and silicone grease. GC-MS evaluation is conducted on products of the first stage at 125 and 135°C, and the second stage products at 145 and 155°C. In the first distillation stage, liquid smoke contains phenol and assorted compounds. Conversely, the second stage yields purer phenol compounds. The findings suggest potential applications of the redistillation product as raw material in food preservation, antiseptics, and insecticides.