A hyphenated method for mercury speciation analysis by the coupling of high performance liquid chromatography and inductively coupled plasma mass spectrometry with the online strong anion exchange column (SAX) preconcentration was developed. The Hg analytes (Hg + , MeHg, EtHg and Hg 2+ ) were absorbed on the SAX column preconditioned with sodium 3-mercapto-1-propanesulfonate, and then rapidly eluted (less than 16s) by 5μL 3% (v/v) 2-mercaptoethanol. The enrichment factors of 1025 for Hg + , 1084 for MeHg, 1108 for EtHg and 1046 for Hg 2+ were obtained using 6mL sample in a 1.5-min enrichment procedure. Rapid separation of the four mercurial compounds was achieved within 5min on a 50-mm C 18 column using 0.5% (v/v) 2-mercaptoethanol as the mobile phase. The detection limits for Hg + , MeHg, EtHg and Hg 2+ were 0.015, 0.010, 0.009 and 0.016ngL −1 , each, and the relative standard deviations of peak height and peak area (5ngL −1 for each Hg species) were all below 5%. Mercury speciation in three freshwater, two drinking water and two seawater samples were then analyzed by the proposed method. MeHg and Hg 2+ concentrations down to 0.14 and 0.56ngL −1 were detected in the drinking waters.