OBJECTIVE: To establish a method for simultaneous determination of 4 effective components in the couple of Coptidis Rhizoma and Evodiae Fructus,and to investigate rational proportion of the couple. METHODS: HPLC method was adopted. The determination was performed on Welch XB C18 column with mobile phase consisted of acetonitrile-1.5 mmol/L sodium dodecyl sulfate solution (pH adjusted to 5.0 with phosphoric acid) (gradient elution) at the flow rate of 1.0 mL/min. The detection wavelength was set at 265 nm, and the column temperature was 30 ℃. The sample size was 10 μL. RESULTS: The linear ranges of berberine hydrochloride, martin hydrochloride, evodiamine and rutacarpine were 2.24-44.80 μg/mL(r=0.999 9), 1.26-31.50 μg/mL(r=0.999 8), 2.70-81.00 μg/mL(r=0.999 8), 1.65-49.50 μg mL(r=0.999 9), respectively. RSDs of precision, stability and reproducibility tests were all lower than 3.0%. The recoveries were 98.11%-100.73%(RSD=1.04%,n=6),96.54%-103.47%(RSD=1.86%,n=6), 95.49%-102.36%(RSD=2.05%,n=6), 97.19%-103.24%(RSD=2.19%,n=6), respectively. When the proportion of Coptidis Rhizoma-Evodiae Fructus(m/m) was 2 ∶ 1, the comprehensive content of each component was the highest. CONCLUSIONS: The method is simple, accurate, stable and reproducible, and can be used for simultaneous determination of 4 effective components in different compatibility proportions of the couple of Coptidis Rhizoma and Evodiae Fructus. The rational proportion of the couple of Coptidis Rhizoma and Evodiae Fructus is 2 ∶ 1.