The invention belongs to the field of analytical chemistry detection, and particularly relates to a liquid chromatography detection method of BC-02. According to the method, methanol-water is taken as a phase A, and acetonitrile-water-trifluoroacetic acid (TFA)-triethylamine (TEA) which is a moving phase is taken as a phase B; due to appropriate proportion adjustment, the requirement of the separation degree of the BC-02 and the adjacent impurity peak can be met, and main degradation products including hydroxymethyl 5-Fu and 5-Fu can be well separated. Under the same chromatographic condition, the method not only is capable of rapidly detecting the content of the BC-02, but also is capable of detecting the isomer of the BC-02 as well as impurities with structures which are the similar to that of the BC-02 at the same time; after the method is used, the proper sample solution concentration is determined, the lower limit of detection is reduced, and quantitative analysis can be well carried out when the concentration of the detected target is lower, so that the detection method has higher practical application values; furthermore, the method is simple and easy to operate, an auxiliary reagent is low in price and easy to obtain, and the detection results are real and reliable; therefore, the method is a rapid and accurate quantitative detection method.