Pressurized liquid extraction, one of the most promising and recent sample preparation techniques, offers the advantages of reducing solvent consumption and allowing for automated sample handling. It is being exploited in diverse areas because of its distinct advantages. However, because the extraction is performed at elevated temperatures using PLE, thermal degradation could be a concern. Z-ligustilide, one of the biologically active components in Angelica sinensis, is an unstable compound, which decomposes rapidly at high temperature. In this study, we carried out a comparative study to evaluate PLE as a possible alternative to current extraction methods like Soxhlet and sonication for simultaneous extraction of Z-ligustilide, Z-butylidenephthalide and ferulic acid in A. sinensis. The operating parameters for PLE including extraction solvent, particle size, pressure, temperature, static extraction time, flush volume and numbers of extraction were optimized by using univariate approach coupled with central composite design (CCD) in order to obtain the highest extraction efficiency. Determination of Z-ligustilide, Z-butylidenephthalide and ferulic acid were carried out by means of high performance liquid chromatography with diode-array detector. The results showed that PLE was a simple, high efficient and automated method with lower solvent consumption compared to conventional extraction methods such as Soxhlet and sonication. PLE could be used for simultaneous extraction of Z-ligustilide, Z-butylidenephthalide and ferulic acid in A. sinensis.