The invention discloses a preparation method of an ultrasonic/fluorescent bimodal microcapsule contrast medium. The method comprises the steps that water-in-oil colostrum which is formed by organic polymer solution and water or aqueous solution under the action of emulsifier is added into polyvinyl acetate (PVA) solution to form emulsion, wherein the at least one type of the organic polymer solution, water or aqueous solution and the PVA solution contains primary amine, at least one type contains aldehyde but does not contain primary amine and aldehyde simultaneously; during a preparation process, the primary amine and aldehyde react to generate a schiff base and produce fluorescent light; after organic solvent is fully volatilized, suspension is washed and freeze-dried and then the contrast medium is prepared. According to the preparation method of the ultrasonic/fluorescent bimodal microcapsule contrast medium, ultrasonic contrast microcapsules are prepared by introducing the in-situ schiff base reaction while preparing the ultrasonic microcapsule contrast medium through a double-emulsion method, and the ultrasonic/fluorescent bimodal microcapsule contrast medium has high fluorescence intensity and good ultrasonic signals. The method has the advantages of convenience in operation, easiness in preparation and extremely good application prospect.