Abstract: OBJECTIVE To establish the quality standard of toad skin sustained-release dropping pills(TSSDP). METHODS TLC testing was used to identify agents in various medicinal materials. The content of cinobufagin and resibufogenin were determined by HPLC. X-ray diffraction and SEM techniques wrer used to study drug statu，and preliminary stability testing were taken. RESULTS Corresponding spots were detected from the sample. The linear range of cinobufagin was 0.002 12-0.012 72 g·L^-1 and resibufogenin was 0.000 44-0.002 64 g·L^-1. They had a good linear relationship, reproducibility and recovery. The drug was possibly dispersed in the matrix with an amorphous state by X-ray diffraction and SEM techniques. The pills had good stability. CONCLUSION This method of quality evaluation is specific, accurate and reliable. It can effectively control the quality of the toad skin sustained-release dropping pills.