Current European legislation demands a reduction in the amount of voltaile organic compounds (VOCs) used in industrial processes. The presence of these compounds in the leather industry arises from the chemicals used in the various stages of the leather manufacturing process. An important aim of tanners is to reduce or eliminate. VOCs, without lowering the quality of their leather products. The HS-SPME-GC-MS method is an innovation in leather analysis. The solid phase micro extration (SPME) is a sample preparation technique used for the extraction of volatile and semi-volatile organic compounds and is becoming widely accepted as the technique of choice for many applications and that can be connected to gas chrompatography. The main advantages of this technique are speed, sensibility, and the fact that it requires no sample handling or solvent extraction. Other advantages include the fact that the concentration and the extraction are reached simultaneously and that it enables on-site extraction of the analyte, even without the prior destruction of the sample. This paper shows the development of a new HS-SPME-GC-Ms method with a deuterated internal standard for the detection and identification of volatile organic compounds emitted by leather. This method enables us to carry out a simple and rapid determination of the qualitative and semi-quantitative composition of the organic compounds in the samples