Objectives: The aim of this work was the quantitative determination of N,N-Dimethylacetamide (DMA) as crystallization solvent in samples of Diacerein.DMA is commonly used as a solvent in the chemical, agricultural and pharmaceutical industries. However, in order to ensure product quality and to protect patients from the potentially toxic properties, the substances used as active ingredients in therapeutic drugs should not contain high levels of residual solvents.Methods: LC is commonly used in the pharmaceutical industry to check DMA in pharmaceutical products, but in this work we were interested in validating and comparing LC/UV and GC/FID techniques for determining the presence of DMA in Diacerein Results: Both methods showed good linearity, precision and accuracy with comparable LOD and LOQ. Conclusion:The GC method, however, since it uses DMSO as an internal standard, has higher analytical versatility, thus allowing the qualitative and quantitative determination of DMA at lower levels than those obtained with LC.