Drinking water treatment plants (DWTP) use chlorination as an oxidation stage in the first step of the processes used to eliminate the natural organic matter (NOM) responsible for the formation of 2-methylisoborneol (2-MIB) and Geosmin (GM), which produce odor and taste to the water. However, chlorination processes give rise to disinfectant toxic subproducts, such as trihalomethanes (THMs). In this work, a headspace solid-phase microextraction coupled with a gas chromatography/mass spectrometric method has been developed for the quality control of drinking water. 2-MIB, GM, and THMs at different stages of the drinking water treatment process were monitored. The method was validated following the Environmental Protection Agency guidelines. Neither carryover nor the matrix effect was observed. The performance of the method was satisfactory in terms of selectivity, repeatability, and accuracy and exhibited a linear concentration range of 0.8–50 µg/L for trichloromethane (TCM), 0.05–20 µg/L for bromodichloromethane, 0.01–20 µg/L for dibromochloromethane and tribromomethane, and 0.005–0.05 µg/L for GM and 2-MIB. The THMs concentration obtained for all the water samples was below the thresholds established by international organizations and, for 2-MIB and GM, were lower for their limit of quantification. The method was also applied to the adsorption kinetic study of TCM on granulated activated carbon, which is the main barrier to reducing the NOM in DWTP.