The conventional Dean–Stark (CDS) distillation is one of the most commonly analytical methods used to determine water content in food products. Toluene is the recommended solvent for this method, but it is also ranked on top of the list of the hazardous solvents despite its concern on safety, environmental and health issues. The aim of this study is to use alpha-pinene instead of toluene (petroleum solvent) for moisture determination in food products using Dean–Stark distillation. The results obtained with the two solvents, alpha-pinene or toluene, were comparable. Statistical tests showed no significant difference between the two procedures used and assessed the efficiency of alpha-pinene Dean–Stark (PDS) method and its reliability. Dean–Stark technique using alpha-pinene could be appropriate for the routine quality control analysis of moisture in food products, but also, easy to handle procedure for lab work students.