Abstract: This paper was aimed at detecting the main pigment in skin of large yellow croaker using reversedphase high performance liquid chromatography(RP-HPLC) with solid phase extraction(SPE). The sample was extracted by acetone and petroleum(v/v=4∶3) ether,and cleaned up by an LC-NH2 column. The chromatographic separation was achieved on a C18column(150mm×4.6mm,5μm) using a mobile phase made up of acetonitrilemethanol(v/v=9∶1) at a flow rate of 1.0m L/min. The detection was performed by a diode detector(DAD) at474 nm. The results showed that lutein,which the proportion was over 50%,was the main pigment in skin of large yellow croake which also contained little amounts of canthaxanthin,astaxanthin and other pigments. An excellent linear relationship of this method for lutein,canthaxanthin and astaxanthin(R2>0.999). The average spike recovery rates of lutein,canthaxanthin and astaxanthin were 84.26% ~96.56%,83.28% ~92.79% and85.61%~94.39% with relative standard deviations of 2.55%~5.78%,3.52%~7.28% and 3.02%~6.55% respectively.The limit of detection was 0.43mg/kg for lutein,0.59mg/kg for canthaxanthin,0.82mg/kg for astaxanthin.