An anal. method for determination of matrine and gallic acid in Compound Liangmianzhen tablets was established by high-performance liquid chromatog. (HPLC). The anal. was achieved on a ZORBAX Eclipse XDB C18 column (250 mm × 4.6 mm, 5 μm) using a mobile phase of acetonitrile-methanol-phosphate buffer (pH 6.8)-triethylamine (16:16:68:0.1) and a mobile phase of acetonitrile-0.1% phosphoric acid and 0.1% triethylamine water solution (3:97), resp. The flow rate was 1.0 mL·min-1, the detecting wavelength was 220 nm, and the column temperature was 30°C. The calibration curve of matrine was linear within the range of 0.10-2.00 μg (r = 0.9996, n = 6), and the average recovery was 99.4% (n = 9). The calibration curve of gallic acid was linear within the range of 0.011-1.75 μg (r = 0.9999, n = 6), and the average recovery was 99.1% (n = 9). The method could be used to control the quality of compound Liangmianzhen tablets.