The aim of this work was to study the combined relationships between biological and chemical parameters with the humification index (HI) and degree of polymerisation (DP) during the composting of a municipal solid waste. During the composting, biological parameters increased during the first 15 days. After the second week, the dehydrogenase, urease, beta-glucosidase, phosphatase and arylsulphatase activities decreased 64%, 50.1%, 49.6%, 24.1% and 58.3%, respectively, compared with their initial values, possibly due to the decreasing of the water-soluble carbon content (WSC). The WSC contents decreased possibly due to the degradation of the microorganisms as carbon and energy sources. The HI increased (66% compared to the initial values) indicating an increase in the structural complexity of the humic substances. The factorial analysis indicates a relationship between the biological properties, WSC and HI and DP. The linear regression analysis indicates the high correlation coefficients found between the HI and DP with chemical and biological properties, and therefore, it can be concluded that combination of chemical and biological parameters can be used to determine the compost maturity.