Abstract: The organic acids in Fructus Mume Concrete were extracted by ASE (accelerated solvent extraction) in dichloromethane-acetonitrile (1:4, v/v) solution, then silanized with N, O-bis(trimethylsilyl)trifluoroacetamide by using trans-2-hexenoic acid and octanedioic acid as internal standards. The method for simultaneous determination of 29 organic acids including formic acid, acetic acid, benzoic acid, hexadecanoic acid, octadecanoic acid, malic acid, citric acid, etc., was developed with GC/MS/SIM. The recoveries ranged from 80.3% to 108.4% and RSDs were all below 10%.