We attempted to develop a direct-injection liquid chromatography/electrospray ionization-tandem mass spectrometry
(LC/ESI-MS/MS) for quantifying chloral hydrate in tap water, for which gas chromatography has been
commonly used. Formic acid and acetonitrile were used as the mobile phase, and the adduct ions [M + HCOO⁻
formed by the interaction between the formate ions and chloral hydrate were detected using the LC/ESI-MS/MS
method. Under these conditions, a simultaneous analytical method was established for chloral hydrate and three
haloacetic acids, the latter of which are Japanese drinking water quality standard items. A spike and recovery test
of the tap water dechlorinated with sodium thiosulfate indicated 88–105 % recovery rates for all components.