OBJECTIVE： To establish a method for content determination of main components and its related substances in Phenzolzine capsules. METHODS： HPLC method was adopted for content determination of main components. The contents of related substance （known impurity 1， known impurity 2， total impurity） were calculated with principle component self-control method. The determination was performed on Inertsil ODS-2 C18 column with mobile phase consisted of acetonitrile-water （55 ∶ 45， V/V）at the flow rate of 1.0 mL/min. The detection wavelength was set at 223 nm， and column temperature was 25 ℃. The sample size was 20 μL. RESULTS： The main component phenzolzine and other impurity peaks were well separated. The liner range of phenzolzine was 20.04-60.12 μg/mL （r＝1.000 0）. RSDs of precision， stability （24 h） and reproducibility tests were all ≤0.5％ （n＝6）. Average recovery was 97.50％ （RSD＝0.36％， n＝3）. The detection limit and quantification limit of phenzolzine were 0.91 ng and 3.04 ng. In 3 batches of samples， average value of phenzolzine， known impurity 1， known impurity 2 and total impurity were 106.68％， 0.002 1％， 0.044 0％ and 0.046 2％， respectively. CONCLUSIONS： Established method is simple， specific， sensitive and accurate for content determination of main component and related substance in Phenzolzine capsules. It is suitable for quality control of Phenzolzine capsules.