A sensitive and selective method for the determination of 4-hydroxycoumarin-type rodenticides (warfarin, coumatetralyl, bromadiolone, and brodifacoum) in animal products, fishery products, and honey was developed. 4-Hydroxycoumarin rodenticides were extracted with acidified acetone, and the crude extract was purified by liquid-liquid partitioning followed by PSA column cleanup. Gradient liquid chromatographic separation was performed by using an Inertsil ODS-4 column, with methanol and water containing ammonium acetate as the mobile phase. Detection was carried out on a tandem mass spectrometer with electrospray ionization in the negative mode. Average recoveries from bovine muscle, bovine liver, bovine fat, swine muscle, salmon, eel, freshwater clam, egg, milk, and honey spiked at 0.0005-0.001 mg/kg were in the range of 79-108%, and the relative standard deviations were 2-8%. The limits of quantitations of the developed method were 0.0005 mg/kg for brodifacoum, 0.001 mg/kg for warfarin, coumatetralyl, and bromadiolone.