An analytical method employing solid phase extraction (SPE) and gas chromatography-tandem mass spectrometry (GC-MS/MS) has been developed for quantitative determination of twenty-six organohalo-gen disinfectant by-products (OXBPs) in water samples. Target analytes include four trihalomethanes (THMs), four iodohalomethanes (I-HMs), one haloacetaldehyde (HAL), six haloketones (HKs), four haloni-tromethanes (HNMs), and seven haloacetonitriles (HANs). The sample preparation procedure includes pretreatment with ascorbic acid to quench residual oxidants, followed by analyte enrichment using solid-phase extraction. Five SPE sorbents were tested. The best results for the majority of target analytes were obtained using a styrene-divinylbenzene copolymer phase and methyl tert-butyl ether (MTBE) as the elution agent. GC-MS analysis was performed using electron ionization (EI) and selected reaction monitoring (SRM) for analyte detection. The performance of the method was assessed according to the French standard NF T90-210. The method showed LOQs ranging from 3 to 3000 ng L −1. The applicability of the method has been demonstrated by analyzing both river water and tap water samples. The OXBPs detected most often in the tap water were dibromochloromethane (in 100% of the samples, 4.3-4.7 g L −1), bro-modichloromethane (100%, 1.3-1.7 g L −1), tribromomethane (100%, 0.8-4.4 g L −1), trichloromethane (100%, 0.6-0.7 g L −1), dibromoacetonitrile (75%, 0.5-0.9 g L −1), with dichloroacetonitrile and 1,1,1-trichloro-2-propanone detected at concentrations around the LOQ levels. In the treated river water samples, the only OXBPs measured at levels above the limit of quantification were trichloromethane and 1,1,1-trichloro-2-propanone. To the best of our knowledge, this is the first SPE-GC-MS/MS method enabling the analysis of an extensive list of OXBPs.