The polyacrylamide hydrogel (PAMG) has been used in cosmetology in China, Ukraine and Russia since 1990s. Because the monomer acrylamide(AM) used to produce PAMG has been implicated as a potential mutagen and reproductive toxicant[1,2], it is important to accurately determine the amount of residual AM monomer in the PAMG. In this study, a quick, practical and simple method to determine AM is presented with respect to the hydrogel. AM is analysed quantitatively by ODS-3 column with ultraviolet (UV) absorbance detector. AM is separated from interferential component with an aqueous solution of 0.9%NaCl (NS) adjusted at pH~3.7 using hydrochloric acid and then detected at a UV wavelength of 210 nm. The results show that ODS-3 is effective approach for quantifying AM concentrations in PAMG. This method has a lower detection limit of 0.003µg/ml and a linear response range of 0.003 and 0.9 µg/ml (depending on the range required for analysis). Precision studies give coefficients of variation of <3.2%(n=5) for 0.003µg/ml. The recoveries for this method are greater than 90%. When AM content in PAMG is lower than the detection limit of this method, SPE (solid phase extraction) could be used to concentrate AM. In the case, C18 cartridge is used. And the recoveries are about 70% for SPE when AM concentration is lower than ppb.