An　easy,　sensitive　and　quick　method　was　established　for　simultaneously　separating　and　determining　stimulant,　narcotics　and　antiestrogen　in　spiked　human　urine　using　gas　chroma-tography-nitrogen　phosphorous　detection　(GC-NPD).　The　urine　sample　was　preprocessed　by　liquid-liquid　extraction.　Tert-butyl　methyl　ether　and　JV-phenylamine　were　chosen　as　extraction　solvent　and　internal　standard　for　quantitation,　respectively.　That　is,　a　standard　stock　mixture　containing　methylephedrine,　meperidine,　methadone,　tamoxifen,　fentanyl　and　N-phenylaniline　was　added　into　5.　0　mL　urine　samples　and　mixed　uniformly;　then　0.　5　mL　5.　0　mol/L　NaOH,　3.　0　g　NaCl　and　5.　0　mL　tert-butyl　methyl　ether　were　added　and　finally　centrifuged.　The　extraction　solution　was　dried　under　N2,　redissolved　by　acetone　and　then　determined　by　GC-NPD.　The　method　showed　the　satisfactory　linearity　was　between　0.022-20　mg/L,　with　the　coefficient　correlation　from　0.　994　5　to　0.　999　8.　The　detection　limits　were　in　the　range　of　0.　007　-0.　015　mg/L,　and　the　average　recoveries　in　spiked　urine　were　between　75.　8%　-　118.　2%　and　the　relative　standard　deviations　were　lower　than　17.2%.