A　novel　method　to　determine　semi-volatile　organic　compound(semi-VOC)　was　established　by　HPLC　coupled　with　a　partly-immersed　three-phase　hollow　fiber　liquid　phase　microextraction　(PI-LPME)　technique　for　sample　preparation.　The　influence　of　extraction　parameters　including　organic　solvent,　pH　of　donor　and　acceptor　phase,　extraction　time,　the　proportion　of　hollow　fiber　in　gas　and　liquid　were　optimized.　Under　the　optimum　conditions,　the　proposed　method　provided　linear　range　of　0.05-10　mu　g/ml　with　r(2)　0.9992,　detection　limit　of　5　ng/ml　(S/N=3),　RSD　＜　5%(n=　5)　and　relative　recovery　of　95.91-97.95%.