顶空气相色谱法测定制药废水中残留有机溶剂韩明活

,,(,511515):。。:SE-5430m×0.53mm×5μm;:40℃,5min,90℃,2℃/min,0min,160℃,30℃/min,2min;:FID;:220℃;:260℃;:;:8ml/min;:10∶1。0.079～1.582mg/ml、0.079～1.576mg/ml、0.081～1.620mg/ml、0.052～1.038mg/ml、0.070～1.410mg/ml。(n=9)100.3%～104.1%。、,。:;;中图分类号:R927　　　　　　文献标志码:A　　　　　　　文章编号:1673-4610(2010)08-0021-02:韩明活,制药工程师,执业药师,Tel:[phone],E-mail:[e-mail]alSolventsinPharmaceuticalWasteWaterbyHeadspaceGasChromatographyHANMing-huo,ZHANGMei-lan,ZHUMin-jie(GuangdongBlueTreasurePharmaceuticalCo.,Ltd,Qingyuan,Guangdong511515,China)Abstract:ObjectiveToestablishamethodforthedeterminationofresidualsolventsinpharmaceuticalwastewater.MethodsHeadspacegaschromatographywasemployed.Chromatographicconditions:SE-54capillarycolumn(30m×0.53mm×5μm)wasused.Columntemperaturewas40℃initiallyandmaintainedforfiveminutes;then,heatedupto90℃attherate2℃/minandmaintainedforzerominute;afterwards,heatedupto160℃attherateof30℃/minandmaintainedfor2min.Flameionizationdetector(FID)wasusedanditstemperaturewas260℃;temperatureoftheinjectorwas220℃.Nitrogenwasusedasthecarrygas;theflowratewas8ml/min;andthedistributaryratiowas10∶1.ResultsThecalibrationcurvesformethanol,acetone,n-butylalcohol,toluene,andbutylacetatewerelinearintheirrespectiverangesof0.079～1.582mg/ml,0.079～1.576mg/ml,0.081～1.620mg/ml,0.052～1.038mg/mland0.070～1.410mg/ml.Theaveragerecoveryrates(n=9)werebetween100.3%～104.1%.ConclusionThismethodiseasytooperatewithpreciseresults,andreliablefordeterminingtheresidualsolventsinpharmaceuticalwastewater.Keywords:headspacegaschromatography;pharmaceuticalwastewater;residualsolvents　　2008-08-01《》,。COD()120mg/L,《》300mg/L,2010-07-01。,,。,,。,,,。1　1.1　1.1.1　仪器　:Agilent6890N,FID,AgilentChemstationRevA.09.03。1.1.2　试药　、(0.791g/ml)、21·20108208·(0.788g/ml)、(0.810g/ml)、(0.865g/ml)、(0.881g/ml),、。1.1.3　对照品溶液制备　500μl(396mg),500μl(394mg),500μl(405mg)300μl(260mg),400μl(352mg)50ml,,。1、2、3、5、10、20ml100ml,,①②③④⑤⑥。:0.079、0.158、0.237、0.396、0.791、1.582mg/ml,:0.079、0.158、0.236、0.394、0.788、1.576mg/ml,:0.081、0.162、0.243、0.405、0.810、1.620mg/ml,:0.052、0.104、0.156、0.260、0.519、1.038mg/ml,:0.070、0.141、0.211、0.352、0.705、1.410mg/ml。1.2　:SE-5430m×0.53mm×5μm;:40℃,5min,90℃,2℃/min,0min,160℃,30℃/min,2min;:FID;:220℃;:260℃;:;:8ml/min;:10∶1。1.3　2ml,,。,。2　2.1　⑤。1.5,8000(1)。1、2。1　(%)-919811.33820928.561443820.78289398.72369442.2　①②③④⑤⑥。(x),(y),(2)。,。1　2　2　(n=6)ry=866x-60.99985y=3719x+40.99964y=2514x+1940.99629y=32028x+5690.99965y=11901x+6650.998412.3　1ml22ml,③、④、⑤1ml,。100.3%～104.1%,3。2.4　⑤,6。RSD5.0%。3　(n=9)(%)RSD(%)100.31.4101.21.2101.61.8103.42.2104.11.92.5　③,,10∶1,4。,。(下转第27页)22PharmacyToday·20108Vol.20No.8·。,0.1%80--,,0.1%80--,100ml,3,2100ml,100cfu;1100ml。。14d,。30～35℃,23～28℃。3　3.1　:,。3.2　,0.1%80-,80,。3.3　,,。80,,。、、,。[1].[M].:,2003:2342-2346.[2].()[S].:,2010:ⅩⅢB,76-79.[3].[S].:,2005:313-323.[4].[J].,2008,9(3):219-221(收稿日期:2010-02-26)(上接第22页)4　(mg/L)0.480.480.480.320.612.6　3,(5)。5　(mg/L)(mg/L)(mg/L)(mg/L)(mg/L)120132610356483　3.1　、、,,,。3.2　,,。3.3　,1.5,8000,。3.4　,2。2,。3.5　。,。[1].()[S].:,2010:31-32,194-195.[2]/.GB/T5750.8-2006—[S].:,2007.[3].[J].,2004,17(2):83-89.(收稿日期:2010-03-31)27·20108208·