Microwave-assisted derivatization for methylmalonic acid analysis in human serum by gas chromatography-mass spectrometry

Analytical methods

Feng Zhu¹  Dagui Zheng¹ 

[1] Key Laboratory of Applied Organic Chemistry, Higher Institutions of Jiangxi Province, Shangrao Normal University,Shangrao,China

DOI  :  10.1039/B9AY00289H

学科分类：分析化学

来源: Royal Society of Chemistry

【 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...

【 授权许可】

CC BY-NC