Huge volumes of wastewater containing organic flotation reagents such as xanthates have been released into the environment via mining activities, greatly threatening the eco-environment safety. A simple and fast method is urgently needed for accurate analysis of various xanthates in mining and environmental water. Here, a robust method is realized for simultaneous determination of three trace xanthates (i.e., potassium ethyl xanthate, potassium butyl xanthate, and potassium isopropyl xanthate) in environmental water samples, including eutrophic water and flotation wastewater using solid phase extraction (SPE) and HPLC-MS/MS. HPLC-MS/MS parameters, SPE cartridges and eluting solvents, pH values, and SPE procedures were optimized. The new method had an excellent linearity in the range of 1-1000 μg/L (R