Pesticide use is permanently increasing for several reasons. However, these chemical compounds are threatening human health and environment. Thus, natural pesticides are recently emerging as an alternative solution. In fact, as these biopesticides are issued from nature, they are supposed less harmful versus the environment. However, the evaluation of biopesticides’ environmental impact remains an actual challenge. In fact, classical methods e.g. half-life are limited, due to the complexity of biocontrol products. Thus, new omics-based methods are being developed in order to adapt new environmental evaluation protocols. In this context, Environmental Metabolic Footprinting (EMF) was recently developed using Liquid Chromatography-Mass Spectrometry (LC-MS) based metabolomics approach [1,2], aiming to introduce the “resilience time” as a new integrative evaluation concept. It corresponds to the time required for the dissipation of the compound and its effect on the matrix microbiome. More recently, a new approach was considered in order to study the volatile compounds in environmental samples. In fact, pesticide degradation can lead to volatile by-products. Moreover, volatile microbial compounds can signalize biodiversity disruptions. Thus, novel Headspace-Solid Phase Micro Extraction-Gas Chromatography-Mass Spectrometry (HS-SPME-GC-MS) based analytical method is being developed, in order to analyze the environmental “Volatilome” (xenovolatilome + microbial volatilome). A kinetic study is performed in order to evaluate the volatilome changes over the time. It could supplement the information given by LC-MS-based EMF. Furthermore, this methodology shows several advantages. In fact, no laborious and complex steps for sample preparation are needed. Therefore, this method reduces time, solvents and chemical reagents consumption, which agrees with green chemistry and reduce analysis coast. Preliminary tests were performed with sediment samples. These sediments were treated with Bacillus thuringiensis israelensis (Bti), a complex bio-insecticide, and the α-Cypermethrin, a standard chemical insecticide. For two days kinetics study (day 0 and day 8), HS-SPME-GC-MS analyses were applied, with no complex extraction needed, as mentioned above. They were followed by unsupervised descriptive multivariate statistical analysis in order to analyze the changes in volatilome. The results demonstrate sufficient sensitivity to discriminate between Bti treated samples and control samples. Moreover, some Variables Importance in Projection (VIP) are detected by supervised explicative multivariate analysis. More optimization is planned to enhance the reliability for complex and long-scale kinetic studies, in order to set a novel, simple and cheap method to be applied in EMF concept. [1]: Patil et al. 2016. Sci. Total Environ. 566–567:552–558 [2]: Salvia et al. 2018. Environ. Sci. Pollut. Res. 25(30):29841–29847