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Abstract: Current research indicates that much of the unidentified fraction of drinking water disinfection by-products (DBPs) is highly polar and of high molecular weight. The combination of liquid chromatography and mass spectrometry (LC–MS) is being increasingly used for the direct analysis of these highly polar, hydrophilic DBPs and for the exploration of high molecular weight by-products. Further, improvements in LC–MS instrumentation and analytical techniques are providing low μg/L and ng/L detection limits, which allow trace levels of DBPs to be measured. This review covers recent applications of LC–MS and other related techniques, such as flow injection-atmospheric pressure chemical ionization and electrospray ionization (ESI)-MS, high-field asymmetric waveform ion mobility spectrometry–ESI–MS, membrane-introduction MS, and ion chromatography–ESI–MS for measuring known DBPs and exploring the nature of previously uncharacterized DBPs. [Copyright &y& Elsevier]