The metabolic investigation of human populations is increasingly important in the study of health and disease. Urinary metabolic profiling plays a significant role in systems biology research, expanding its applications in clinical diagnostics, mechanistic studies, personalized health care, and molecular epidemiology. This study underscores the importance of analyzing volatile organic compounds (VOCs) using advanced characterization instruments, particularly for diagnosing colorectal cancer. Early detection through screening is crucial for effective treatment and improved prognosis in colorectal cancer, a prevalent malignancy characterized by abnormal cell growth in the colon or rectum, often detectable through biomarkers in urine. An in-depth quantitative study was conducted using a cohort of urine samples from colorectal cancer patients and non-cancer controls, employing Gas Chromatography-Ion Mobility Spectrometry (GC-IMS).