A rapid, sensitive and reproducible high performance liquid chromatography (HPLC) method with post-column fl uorescence derivatization has been developed to determine the amount of low-molecularweight sulfated polysaccharide (GFS) in vivo . The metabolism of GFS has been shown to fi t a two component model following its administration by intravenous injection, and its pharmacokinetic parameters were determined to be as follows: half-time of distribution phase ( t 1/2α )=11.24±2.93 min, half-time of elimination phase ( t 1/2β )=98.20±25.78 min, maximum concentration ( C max )=110.53 μg/mL and peak time ( T max )=5 min. The pharmacokinetic behavior of GFS was also investigated following intragastric administration. However, the concentration of GFS found in serum was too low for detection, and GFS could only be detected for up to 2 h after intragastric administration (200 mg/kg body weight). Thus, the bioavailability of GFS was low following intragastric administration because of the metabolism of GFS. In conclusion, HPLC with postcolumn derivatization could be used for quantitative microanalysis and pharmacokinetic studies to determine the presence of polysaccharides in the serum following intravenous injection.