Rapid hemostasis, biosafety, and adaptability to different bleeding sites are the focus of research on hemostatic materials. In this work, an efficient and simple preparation of aldehyde starch hemostatic microspheres (ASHMs) crosslinked with L-cystine dimethyl ester was developed. Through a series of physicochemical parameters and in vitro and in vivo hemostatic properties measurements, the results showed that under the optimal crosslinking degree, ASHMs had a regular and uniform spherical shape, and it had a liquid suction capacity of up to 880%. At the same time, the aldehyde groups on its surface can increase the adhesion and aggregation of blood cells, thereby enhancing the hemostatic effect, which can be considered as a synergistic effect. More importantly, ASHMs have good biocompatibility and minimal intradermal irritation. Taken together,ASHMs could be used as potential novel hemostatic materials for surgical treatment.