Abstract This study addresses the growing need to accurately identify trace elements in the environment, an important factor in effective pollution control and protection of public health. The goal was to evaluate and compare the sensitivity, selectivity, and specificity of Gas Chromatography-Mass Spectrometry (GC-MS) and Liquid Chromatography-Mass Spectrometry (LC-MS) of different environmental matrices such as air, water, soil, and wastewater. Controlled laboratory experiments were carried out to assess the effectiveness of both techniques for the detection of polycyclic aromatic hydrocarbons (PAHs), volatile organic compounds (VOCs), chemicals, and pesticides. Results revealed that GC-MS achieved high sensitivity for VOCs in air, with detection limits reaching of 0.1 pg/mL, and for PAHs in water and soil, with detection limits down to 2 pg/g. However, GC-MS performance was reduced in complex matrices like soil due to matrix effects. Conversely, LC-MS excelled in detecting polar and non-volatile compounds, such as pharmaceuticals in wastewater, reaching detection limits down to 0.5 pg/mL, and pesticides in soil, with detection limits down to 2 pg/g, even while contending with challenges like ion suppression. The findings emphasise the need to select an analytical method based on analyte type and matrix complexity to ensure precise detection and reliable results in complex environmental samples.