A method involving the simultaneous extraction and separation of 12 organochlorine pesticides (OCPs) from Angelicae sinensis was developed using supercritical fluid extraction (SFE). The pesticides in the study were alpha-, beta-, gamma- and delta-benzene hexachloride, PCNB (pentachloro- nitrobenzene), PCA (pentachloroaniline), HEPT (heptachlor), MPCPS (methyl-pentachlorophenyl sulfide), pp'-DDE [1,1-dichloro-2,2-bis (p-chlorophenyl) ethylene], op'-DDT [1,1,1,-trichloro-2-(o-chlorophenyl)-2-(p-chlorophenyl) ethane], pp'-DDD [1,1-dichloro-2,2-bis(p-chlorophenyl) ethane], and pp'-DDT [1,1,1,-trichloro-2,2-bis (p-chlorophenyl)ethane]. The extraction conditions were optimized as follows: pure CO(2), extraction pressure 15 MPa, extraction temperature 60 degrees C, extraction time 20 min, and flow-rate 1.5 mL/min. A GC method with electron capture detection was employed to determine the OCPs in Angelicae sinensis. An HPLC method was developed for the quantitative determination of active constituents. The SFE provided high decontamination rate of OCPs and low loss of active constituents in Angelicae sinensis.