Abstract: Polyprenols(C75-C110)of purity over 87.2% were separated and prepared from leaves of Gingkgo biloba L. Polyprenyl phosphate dichlorate was synthesized by choosing phosphorus oxychloride (POCl3) as phosphate,and was converted into polyprenyl phosphate with triethanylamide as hydrolytic reagent with yield more than 65%.The molar ratio of polyprenols to POCl3 was 1:5-10.Phosphate ester reaction temperature was below 10℃,and hydrolysis for 20 h at room temperature.The hydrolysate was purified by silicon gel chromatography and polyprenyl phosphate was obtained by HPLC,and its chemical structure was identified as polyprenyl monophosphate with IR,1HNMR,13CNMR and HRMS.