Objective:To establish a method for simultaneous determination of isovanillin,periplocin and 4-methoxy salicylaldehyde in Cortex Periplocae.Methods:The analysis was performed on a Hypersil ODS2 column (250 mm 4.6 mm,5 μm).The mobile phase consisted of acetonitrile (A) and 0.02% aqueous phosphoric acid (B),with gradient program adopted as follows:0-10 min,85%B;10-40 min,85%B→70%B;40-60 min,70%→50%B.The flow rate was maintained at 1.0 mL·min-1 and the detection wavelength was set at 230 nm.Results:The linear response ranges were 1.65-13.7 μg·mL-1 for isovanillin (r=0.9996),5.91-49.2 μg·mL-1 for periplocin (r=0.9994) and 4.97-99.4 μg·mL-1 for 4-methoxy salicylaldehyde (r=0.9996).The recoveries (n=9) of these compounds were 101.7%,99.5% and 99.9%,respectively.Conclusion:The method is simple,accurate and reproducible for quality control of Cortex Periplocae.