A simple, sensitive, and precise method for the determination of Taxol,® cephalomannine, and 7‐epi‐taxol in Taxus by solid phase extraction followed by high performance liquid chromatography (HPLC) was developed. In this paper, we describe the use of a novel high molecular resin (PRP‐6) as the loading material in the solid phase extraction column to pretreat the digestion solutions of Taxus. The variables affecting the separation and determination were investigated in detail. Under the selected optimal conditions, Taxol, cephalomannine, and 7‐epi‐taxol in Taxus were determined; the recoveries were in the range of 92.6%–110.9%, RSD were in the range of 4.9%–6.3%, the detection limits were 0.1 µg mL−1. These results can be considered satisfactory.