Derivatization of β‐dicarbonyl compound with 2,4‐dinitrophenylhydrazine to enhance mass spectrometric detection: application in quantitative analysis of houttuynin in human plasma

作者: Xiaotao Duan , Dafang Zhong , Xiaoyan Chen

DOI: 10.1002/JMS.1382

关键词: Mass spectrometryTandem mass spectrometry2,4-DinitrophenylhydrazineChemistryDerivatizationAntibacterial agentHigh-performance liquid chromatographySelected reaction monitoringChromatographyLiquid chromatography–mass spectrometry

摘要: Houttuynin (decanoyl acetaldehyde), a beta-dicarbonyl compound, is the major antibacterial constituent in volatile oil of Houttuynina cordata Thunb. In present work, detection houttuynin human plasma based on chemical derivatization with 2,4-dinitrophenylhydrazine (DNPH) coupled liquid chromatography/tandem mass spectrometry was described. The primary reaction products between compound and DNPH aqueous phase were identified as heterocyclic structures, which spectrometric ionization fragmentation behavior characterized aid high-resolution multistage spectral analysis. For quantification, internal standard (IS, benzophenone) firstly converted to their derivatives without sample purification, then extracted from n-hexane detected by chromatography tandem performed selected monitoring (SRM) mode. This method allowed for lower limit quantification (LLOQ) 1.0 ng/ml using 100-microl plasma. validation results showed high accuracy (%bias < 2.1) precision (%CV 7.2) at broad linear dynamic range (1.0-5000 ng/ml). simple quantitative analysis facilitates sensitive robust determination pharmacokinetic studies.

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