A　new　method　based　on　SPE-RPLC-FLD　was　established　for　the　quantitative　determination　of　total　NPnEO　in　wastewater.　The　sample　was　pretreated　using　SPE　column　of　Oasis((R)　HLB　in　Waters　Corporation.　The　column　was　eluted　by　6mL　of　90%　dichloromethane　in　methanol(v/v),　and　the　eluting　liquid　was　volatilized　to　I　ml　capacity　under　breezing　nitrogen　gas　current.　The　recovery　of　the　process　is　99.68%.　NPnEO　in　the　sample　were　separated　by　the　Agilent　1100　LC　instrument　with　ZORBAX　Eclipse　XDB　C-18　liquid　chromatography　column　and　with　the　mobile　phase　of　methanol　and　water　at　the　flow　rate　of　1.0mL　per　min.　Gradient　elution,　the　proportion　of　methanol　in　water　is　increased　from　70%　to　1001/o　gradually　at　2.5　%　per　min,　was　applied　to　the　process.　The　oven　temperature　is　set　at　23　degrees　C,　and　injection　volume　is　15　mu　L.　The　component　signals　were　detected　by　FLD　with　313nm　excitation　wavelength　and　230nm　emission　wavelength.　External　standard　calibration　method　was　chosen　as　quantitative　analysis.　Above　90%　recovery　of　NPnEO　was　checked　up　by　analyzing　real　sewage　and　additional　sample　using　the　method,　and　RSD　was　below　10%.　The　LOD　of　the　method　for　NPnEO　was　fro　m　0.097　to　0.190　microgrammes　per　liter.　NPnEO　concentration　of　some　samples,　including　raw　sewage,　effluent　of　biotreatment　system　and　reclaimed　water,　was　analyzed　by,bis　method.　The　results　show　that　the　accuracy　and　precision　of　the　method　were　satisfactory.