搜索
1988－。*E－mailmeiyong2006@163．com【】*4300653。watersC18+0．1%33+670．7ml/min230nm。325μg/ml～1000μg/mlr0．9995～0．99962．0%～9．6%91．36%～101．36%2－、3－4－0．47μg/ml、0．46μg/ml、0．41μg/ml3－4－。3－4－－。O657．7+2A1004－8685201303－0547－04StandardizedstudyonthedeterminationofmethylhippuricacidsinurinebyHPLCLIUJieMEIYong*WANGYa－nanGUYing－yingWANGQianJIANGJin－fengMedicalCollegeWuhanUniversityofScienceandTechnologyWuhan430065ChinaAbstractObjectiveTogetabetterseparationofmethylhippuricacidisomersandestablishastandardizedmethodforthedeterminationofmethylhippuricacidsinurinebyHPLC．MethodsC18columnwasusedtodeter-minethemethylhippuricacid．ThemobilephasewasMethanol－0．1%aceticacid33∶67．Thedetectorwasper-formedatλ=230nmat0．7ml/min．ResultsCalibrationcurvesofthreemethylhippuricacidswerelinearintherangeof25μg/ml～1000μg/mlwithacorrelationcoefficientmorethan0．999．Theaveragerecoverywasintherangeof91．36%～101．36%andtheaverageRSDwasintherangeof2．0%～9．6%．Theminimumdetectioncon-centrationsof2－MHA3－MHA4－MHAwererespectively0．47μg/ml0．46μg/ml0．41μg/ml．Thesepa-rationof4－methyhippuricacidand3－methyhippuricacidwasupto1．44．ConclusionThemethodisabletomake3－methylhippuricacidand4－methylhippuricacidbaselineseparatedandthemethodologyindicatorsareinlinewiththerelevantrequirementsofthemethodfordeterminationofchemicalsintheoccupationalhealthstandard－settingGuidePartV．Soitcanbeusedtodeterminemethylhippuricacidsinurineofxylenesexposureworkers．KeywordsHPLCMethylhippuricacidIsomerStandardizedstudyXylenes、、、、。、3395%2－、3－4－1。。322012ACGIH1．5g/g32008DFG2．0g/L。4WS/T53－19964－3－56。4－3－774520133233ChineseJournalofHealthLaboratoryTechnologyMar2013Vol23No3。11．1Waters2695Waters2998KQ－500EDK－450BKFBS21SsartoriousTDL80－2BWH－3。2－2－MHA、3－3－MHA4－4－MHASigmaAldrichSteinheimGermany0．1%0．45μm30min。1．21．2．1watersC185μm150mm×4．6mm+0．1%33+67230nm0．7ml/min10μl35℃。1．2．2325．0mg25ml1000μg/ml。25μg/ml、50μg/ml、100μg/ml、200μg/ml、500μg/ml、1000μg/ml1．2．3。1．2．31．0ml10ml0．1ml1+1、0．3g4ml1min5000r/min5min。0．4ml70℃。1．0ml。1．2．4。1．2．5C=c×kC－mg/Lc－μg/mlk－。22．13－、4－233nm、239nm2－190nm～500nm64254nm233nm、239nm、254nm、230nm4230nm4－3－。2．24－3－。0．5ml/min～1．0ml/min4－、3－0．7ml/min。2．30．1%0．1%20∶8040∶603－4－R、tr133∶67。1Rtr2．4。125μg/ml～1000μg/ml。12－y=3802x+2049r=0．99963－y=8601．2x－20910．6r=0．99954－y=6977．1x－9093．3r=0．9995284520133233ChineseJournalofHealthLaboratoryTechnologyMar2013Vol23No332．510。C=3×s×ccC－μg/mls－μg/mlc－μg/mlc－μg/ml1010μg/ml32－2－MHA、3－3－MHA4－4－MHA0．47μg/ml、0．46μg/ml、0．41μg/ml。2．63。463、、350μg/ml300μg/ml800μg/ml3。32。2μg/mlμg/ml%RSD%2－5050．27100．532．7300304．09101．362．9800781．5197．699．63－5048．9297．846．7300303．53101．172．9800792．3899．048．64－5045．6891．362．0300303．9101．32．8800801．6100．26．92．7。100μg/ml200μg/ml400μg/ml。2．83300μg/ml46“1．2．3”4℃。、3、7、14。≤10%。34℃14。R=m1－m2m1×100%m1μg。m2μg。32－MHAX±SDμg/mlR%3－MHAX±SDμg/mlR%4－MHAX±SDμg/mlR%297．70±2．16302．53±2．19298．56±2．733296．85±2．600．28300．98±2．870．5297．15±2．590．477290．96±5．322．26298．07±5．491．47295．40±5．681．0514285．63±5．884．06290．43±6．863．99289．05±6．193．182．921578hTWA0．97mg/m3～144．21mg/m324．19mg/m3±8．50mg/m320．0mg/L～2246mg/L4。20。94520133233ChineseJournalofHealthLaboratoryTechnologyMar2013Vol23No34MHAmg/m3mg/m3Mean±SDRangeMHAmg/LMean±SDRange＜50499．87±11．630．97～49．9385．0±56．120．0～25950－100663．57±12．2850．84～79．63192±25726．1～199≥1002138．96±7．43133．71～144．211728±7331210～22463－0．1%33+673－4－－3。1．－M．2．2006153－155．2CaporossiLDeRosaMPapaleoB．CompleteseparationofurinarymetabolitesofxyleneinHPLC/DADusingβ－cyclodextrinApplica-tionforbiologicalmonitoringJ．JChromatogrBAnalytTechnolBi-omedLifeSci20108782726112615．3ACGIH．TLVsandBEIsbasedonthedocumentationofthethresholdlimitvaluesforthechemicalsubstancesandphysicalagentsandbiolog-icalexposureindicesS．ACGIHCincinnati2012110－111．4WS/T53－1996．、S．5．、J．200824171777－1778．6．、J．2010377245－246．7GBZ/T210．5－2008．S．2012－08－315463、。50．2μg/L。88．9%0%。10%。。－、。1．、J．200919102459－2460．2．J．20082345－6．3．J．2007172258－260．4．J．2011233255－260．5．－J．201230111094－1099．2012－10－1005520133233ChineseJournalofHealthLaboratoryTechnologyMar2013Vol23No3