Microwave-assisted derivatization for methylmalonic acid analysis in human serum by gas chromatography-mass spectrometry
[摘要] Methylmalonicacid(MMA)inhumanserumisanimportantbiomarkerofmethylmalonicacidemias.Inthiswork,asimpleandfastmethodbasedonmicrowave-assistedderivatization(MAD)followedbygaschromatography-massspectrometry(GC-MS)wasdevelopedforthedeterminationofmethylmalonicacidinserum.Intheproposedmethod,theMMAwasextractedfromserumandrapidlyderivatizedwithbis(trimethylsilyl)trifluoroacetamideundermicrowaveirradiation,finallythederivativewasanalyzedbyGC-MS.Theexperimentalparameterswereinvestigatedandthemethodvalidationswerestudied.Theoptimalconditionswereobtained:50μLofbis(trimethylsilyl)trifluoroacetamideplus1%trimethylchlorosilane(BSTFA-TMCS(99 : 1))asderivatizationregent,microwavepowerof400Wandirradiationtimeof2min.Theproposedmethodprovidedsatisfactoryprecision(RSD2.3–4.5%),widelinearrange(0.021–5mM),goodlinearity(R2>0.999),andgoodrecovery(96–101.3%).TheproposedmethodwassuccessfullyappliedtotheanalysisofMMAinserumsamples.Theexperimentalresultsshowedthattheproposedmethodwasasimple,rapid,andefficienttechniqueforthequantitativedeterminationofMMAinserum...
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[效力级别] [学科分类] 分析化学
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