The invention relates to a preparing method for separating huperzine A from Huperzine Serrate by using high-speed countercurrent chromatograph (HSCCC), which comprises a solvent system for preparing a upper phase of stationary phase and a lower phase of mobile phase. The solvent system comprises normal alkanes of normal heptane, hexane or normal pentane, fatty alcohols of methanol, etanol, normal butyl alcohol or acetone, and water, and the three parts have the following proportions by volume: 1 to 5 portions of normal alkane, 0.1 to 2 portions of fatty alcohol, and 1 to 5 portions of water. The conditional temperature is 20 DEG C to 30 DEG C, a column is filled with stationary phase, the rotary speed of a host machine is 600 to 1000 rpm, and the mobile phase is pumped into the column at a flow speed of 0.5 to 4 mL/min. After the system shows a state of dynamic balance, sample introduction is carried out from a sampling valve, and target ingredients are received according to a monitor. Crystallization is carried out after fraction, concentration and evaporation to dry, and monomers of huperzine A are finally obtained.
