Abstract: This research utilizes a HPLC-UV method for determining the mass fractions of diosbulbin B and catechin in Rhizoma Dioscoreae Bulbiferae combined with different proportions of Radix Angelicae Sinensis. Linearity was obtained over the concentration range of 10~200 μg/mL for diosbulbin B, and 200~1 200 μg/mL for catechin. The average percent recovery of diosbulbin B was 89.4%, and 92.8% for catechin. The contents of diosbulbin B in Rhizoma Dioscoreae Bulbiferae and different combinations (1:1, 1:2, 2:1) with Radix Angelicae Sinensis were 2.90, 1.01, 2.19, 2.04 mg/g, respectively. The contents of catechin were 0.78, 0.35, 0.30, 0.43 mg/g in combinations the same as above. The results suggest that different combination of Rhizoma Dioscoreae Bulbiferae and Radix Angelicae Sinensis would decide different levels of marker components in Rhizoma Dioscoreae bulbiferae, which might be relevant to the efficacy enhancement or toxicity decrease.