Understanding the VOC profile released during the early post-mortem period is essential for applications in training human remains detection dogs and urban search and rescue operations (USAR) to rapidly locate living and deceased victims. Human cadavers were sampled at the UQTR morgue within a 0–72 h post-mortem interval. VOC samples were collected from the headspace above the cadavers, using Tenax TA/Carbograph 5TD dual sorbent tubes, and analyzed using GC×GC-TOFMS. Multiple data processing steps, including peak table alignment and filtering, were undertaken using LECO ChromaToF and custom scripts in R programming language. This study identified 104 prevalent VOCs, some of which are linked to human decomposition, while others are connected to the persistence of living scent. Principal Component Analysis (PCA) further highlighted that VOC profiles can change dynamically over time, even in a controlled setting. The findings underscore the complexity and variability in VOC profiles during the early post-mortem period. This variability is influenced by multiple factors including the individual’s biological and physiological conditions. Despite the challenges in characterizing these profiles, the identified VOCs could potentially serve as markers in forensic applications. The study also highlights the need for additional research to build a dataset of VOCs for more robust forensic applications.
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