OBJECTIVE To establish a HPLC method for measuring the concentrations of the main components in cardioplegic solution. METHODS The contents of K~+, Ca~(2+), Mg~(2+) in the cardioplegic solution were determined by HPLC with Alltech Universal Cation column (100 mm×4.6 mm) and ion detector. The mobile phase was 5 mmol·L~(-1) hydrochloric acid. The flow rate was 1.0 mL·min~(-1). RESULTS Calcium, magnesium and procaine in cardioplegic solution were well separated. The linear correlation of the potassium calibration curve was excellent (r=0.999 8) within the range of 12.00~28.00 μg·mL~(-1), and the average recovery was 101.1% with repeatability RSD of 1.59% (n=6). The linear correlation coefficient of the magnesium calibration curve was 0.999*!7 within the range of 12.00~28.00 μg·mL~(-1), and the average recovery was 101.1% with repeatability RSD of 1.94% (n=6). The linear correlation coefficient of the calcium calibration curve was 0.992*!5 within the range of 2.40~5.60 μg·mL~(-1), and the average recovery was 100.8% with repeatability RSD of 2.00% (n=6). CONCLUSION This method is simple, quick and accurate, and is promising to be used in the quality control procedure for cardioplegic solution.