The anisaldehyde dimethyl acetal (p-MBDMA) that produced by direct electrochemical oxidation synthesis in the anhydrous KF-CH3OH system is easily hydrolyzed in water.The study results indicated that p-MBDMA could be hydrolyzed into anisaldehyde raidly and completely in the acidic mixed solution of methanol,acetonitrile and water.Based on this,a high performance liquid chromatographic (HPLC) method was developed for the determination of p-MBDMA indirectly.The best mobile phase was a mixture of water-methanol-acetonitrile(50∶30∶20,adjusted pH 3.0 by phosphoric acid).The internal mechanism of p-MBDMA in the column was also investigated.The results showed that HPLC method could be successfully applied in the rapid determination of p-MBDMA content.