High purity apigenin(AP) was prepared by antisolvent recrystallization method from old Adinandra nitida leaves. The procedure was as follows: Adinandra nitida leaves were extracted by boiling water, and the extracting solution was hydrolyzed with sulfuric acid to obtain crude apigenin(58.9%); the purity of crude apigenin was further improved by antisolvent recrystallization method. A satisfactory purity(98.47%) and yield(86.65%) was obtained under the optimum purifying condition. Scanning electronic microscopy(SEM),differential scanning calorimetry(DSC), Fourier transform infrared spectroscopy(FTIR) and HPLC-MS/MS were investigated.