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The present invention relates to the preparation methods of a kind of high-purity Paeoniflorin and Albiflorin, including:(1) the Paeoniaceae plant material by smashed containing Paeoniflorin and Albiflorin, is added ethanol solution, ultrasonic extraction, and concentrated extracting solution obtains medicinal extract; Medicinal extract is dissolved with water, extracts, is concentrated under reduced pressure to give extract; (2) column chromatography is used, using macroreticular resin as filler, alcohol solution elutes above-mentioned extract, collects the fraction containing Paeoniflorin and Albiflorin, is concentrated, and it is dry, obtain crude extract; (3) above-mentioned crude extract is separated using high-speed countercurrent chromatography, the solvent system of high speed adverse current chromatogram is made of carbon trichloride, butanol, first alcohol and water;UV detector on-line monitoring is collected fraction and is concentrated under reduced pressure, crystallizes, dry, obtains Paeoniflorin and albiflorin.Paeoniflorin and Albiflorin are prepared using the present invention, product purity is high, and quality is good, is suitable for various model high-speed counter-current chromatographs, is easy to industrialization amplification.