固相萃取气质联用测定水中邻苯二甲酸酯类物质王磊

固相萃取气质联用测定水中邻苯二甲酸酯类物质王　磊1,　张　睿1,　程爱华1,2,　史新斌1,　张　莉1,　王志盈1(1.西安建筑科技大学环境与市政工程学院,陕西西安710055;2.西安科技大学地质与环境工程系,陕西西安710054)　　　:　采用固相萃取预处理和气质联用对5种典型邻苯二甲酸酯类物质(PAEs)进行了测定,针对影响固相萃取的主要因素进行了正交试验,得到了最佳萃取条件(洗脱剂为二氯甲烷,洗脱速率为2.0mL/min,洗脱体积为4mL,水样流速为5mL/min),并确定了5种PAEs的线性范围、线性相关性及最低检出限。该检测方法线性相关性较好,精度高,准确性好,适于水中痕量PAEs的测定。　　:　内分泌干扰物;　邻苯二甲酸酯;　固相萃取;　气质联用:TU991.2　　:C　　:1000-4602(2007)14-0086-04DeterminationofPhthalateEstersinWaterbySolid-phaseExtractionandGC-MSWANGLei1,　ZHANGRui1,　CHENGAi-hua1,2,　SHIXin-bin1,　ZHANGLi1,　WANGZhi-ying1(1.SchoolofEnvironmentalandMunicipalEngineering,Xi’anUniversityofArchitectureandTechnology,Xi’an710055,China;2.DepartmentofEnvironmentalandGeologicalEngineering,Xi’anUniversityofScienceandTechnology,Xi’an710054,China)　　Abstract:　Thesolid-phaseextraction(SPE)pre-treatmentandGC-MSwereusedtodeterminefivephthalateesters(PAEs)inwater.TheorthogonaltestofthemainfactorsinfluencingSPEwascar-riedou.tTheoptimizedextractionconditionsofusingdichloromethaneaselutingsolvent,elutingrateof2.0mL/min,elutingsolventvolumeof4mLandflowrateof5mL/minwereobtained.Thelinearrange,linearrelativityandminimumdetectionlimitsoffivePAEswerealsodetermined.Thismethodhasbetterlinearrelativity,highprecisionandgoodaccuracy.ItadaptstodeterminethetracePAEsconcen-trationinwater.　　Keywords:　endocrinedisruptors;　phthalateesters;　solid-phaseextraction;　GC-MS　　:(50578131);　(94003);　(2005E240)　　(Phthalateesters,PAEs),、、,,[1]。,8623　1420077　　　　　　　　　　　　CHINAWATERWASTEWATER　　　　　　　　　　　　　Vo.l23No.14Ju.l2007,,、。,(DEP)、(DBP)、(DCHP)、(DOP)、(DEHP)5,5PAEs、,。1　试验部分1.1　:、、DEP、DBP、DCHP、DOP、DEHP、Na2SO4、、、、、(),(99.999%)。:SupelcoVisiprepTMDL、KL512、C18、、、、、。1.2　1.2.1　①　:100μL1000mg/L,10mL。,,。②　:、4mL,2min,,。③　:60kPa。④　:20mL,C18,5min。⑤　:,。⑥　:1cmNa2SO4,。⑦　:KL512,,1mL,。1.2.2　,。:40℃1min,4℃/min120℃10min,6℃/min270℃。250℃,GC200℃,5μL,,:0.05mL/min31min,1.0(mLmin-1)/min0.8mL/min,22min;2.0(mLmin-1)/min1.5mL/min25min。TraceMS:EI+,,30～500amu,150μA,70eV,NIST98。2　结果与讨论2.1　5PAEs,5PAEs1。1　PAEsFig.1　DeterminationresultofPAEsbyGC-MS1,4DEP、DBP、DCHP、DOPDEHP,DOPDEHP,,。2.2　①　C18,,、、、,3mL/min、1.0mL/min、4mL,87　,:23　14。1。1　5PAEsTab.1　RecoveryoffivePAEsbydifferentelutingsolvents%DEPDBPDCHPDOP/DEHP10.732.750.355.114.487.6101.593.124.4105.954.0103.01.0313.722.845.6　　1,5PAEs,,。②　、、[2],L9(33)(2),。3,4。3,95PAEs,,5mL/min、2mL/min、4mL。,。2　PAEsTab.2　OrthogonaldesignofPAEs/(mLmin-1)/(mLmin-1)/mL120.52221.04322.06430.54531.06632.02750.56851.02952.043　PAEsTab.3　RecoveryofPAEsinorthogonaltest%DEPDBPDCHPDOP/DEHP127.555.3569.6468.64223.1169.6382.7083.02319.2298.2687.0498.34412.51108.9492.6296.06510.2787.3579.4194.7464.23105.8795.06124.11728.35115.4287.1787.34838.46120.7665.62123.25972.13117.6686.3599.954　PAEsTab.4　AnalyticalresultsofPAEsrecoveryDEPDBPDCHPDOP/DEHP23.0343.5419.9226.065.6714.2321.2129.69.819.2313.6116.092.3　,0.001、0.01、0.05、0.1、0.5、1、5、10、50mg/L,,。5μL,3,YX。1mg/L:5μL,。　CL=(2Nd×C×5)/(H×V)(1)　CL———,g/mL　C———,g/mL　Nd———,mm　H———,mm　V———,μL5PAEs、5。5　5PAEs、、Tab.5　Regressionequation,relativecoefficient,linearrangeandlimitofdetectionoffivePAEs(R2)/(mgL-1)/(mgL-1)/(μgL-1)DEPY=3×106X+1984160.99820.05～100.030.06DBPY=3×106X+30000000.99780.5～50.030.06DCHPY=3×106X+694390.99950.05～50.010.02DOP/DEHPY=3×106X+10000000.98060.05～50.0050.018823　14　　　　　　　　　　　　　　　　　　　　　　　　　　　　5,DBP,5PAEs0.05～5mg/L,51～5mg/L,GC-MSPAEs,。,———,。2.4　100μL0.002mg/L500mL,500μL0.010mg/L500mL。3,,6。6　Tab.6　Precisionandaccuracyoftestmethod%0.002mg/L0.010mg/LDEPDBPDCHPDOPDEHPDEPDBPDCHPDOPDEHP1#80.111696.273.173.183.453.792.861.561.52#71.692.3101.478.578.592.158.797.359.859.83#74.8103.295.867.367.386.854.689.259.359.375.5102.797.873.073.087.455.693.160.260.25.76.13.17.67.65.02.44.31.91.9　　6,0.002mg/L5PAEs70%～102%,,GC-MSPAEs、,。2.5　()PAEs,2006120、420、720PAEs,PAEs,7。,5,。7　PAEs(n=5)Tab.7　ConcentrationofPAEsinrawwaterofawaterworksinXi’an(n=5)DEPDBPDCHPDOPDEHP/(μgL-1)RSD/%/(μgL-1)RSD/%/(μgL-1)RSD/%/(μgL-1)RSD/%/(μgL-1)RSD/%20061200.48521.426NDND0.8060.80620064200.42428.264NDND0.7580.75820067200.38619.327NDND0.6990.699　:　ND。　　7,PAEs,PAEs,DBP,28μg/L。,PAEs。3　结论,:2.0mL/min、4mL、5.0mL/min。51～5mg/L,,0.06μg/L,7.6%,,。,、,PAEs。:[1]　,,.———[J].,2003,25(10):286-288.[2]　,,,.[J].,2000,21(2):66-69.:[phone]E-mail:[e-mail]@163.com:2007-01-0189　,:23　14