In the past 10 years, trends in analytical chemistry have turned toward the green chemistry which endeavours to develop new techniques that reduce the influence of chemicals on the environment. The challenge of the green analytical chemistry is to develop techniques that meet the request for information output while reducing the environmental impact of the analyses. For this purpose petroleum-based solvents have to be avoided. Therefore, increasing interest was given to new green solvents such as limonene and their potential as alternative solvents in analytical chemistry. In this work limonene was used instead of toluene in the Dean–Stark procedure. Moisture determination on wide range of food matrices was performed either using toluene or limonene. Both solvents gave similar water percentages in food materials, i.e. 89.3 ± 0.5 and 89.5 ± 0.7 for carrot, 68.0 ± 0.7 and 68.6 ± 1.9 for garlic, 64.1 ± 0.5 and 64.0 ± 0.3 for minced meat with toluene and limonene, respectively. Consequently limonene could be used as a good alternative solvent in the Dean–Stark procedure