Chromatographia

, Volume 70, Issue 5–6, pp 775–781 | Cite as

Analysis of Hexanal and Heptanal in Human Blood by Simultaneous Derivatization and Dispersive Liquid–Liquid Microextraction then LC–APCI–MS–MS

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Abstract

A new analytical approach, simultaneous derivatization and dispersive liquid–liquid microextraction followed by liquid chromatography–atmospheric-pressure chemical ionization tandem mass spectrometry, has been developed for analysis of hexanal and heptanal in human blood. In the derivatization and extraction procedure a solution of 2,4-dinitrophenylhydrazine (derivatization reagent) in 85 μL acetonitrile (dispersive solvent) and 50 μL tetrachloromethane (extraction solvent) was rapidly injected into the aqueous sample containing hexanal and heptanal. Within a few seconds the aldehydes were derivatized and simultaneously extracted. After centrifugation, the hydrazones in the sediment phase were analyzed by LC–APCI–MS–MS. Derivatization and extraction conditions were investigated systematically. Under the optimum conditions enrichment factors for hexanal and heptanal in a 1-mL sample were 63 and 73, respectively. The calibration plots were linear in the ranges 0.5–100 and 100–1,000 nmol L−1, respectively, and the respective limits of detection (LOD) were 0.17 and 0.076 nmol L−1. Reproducibility and recovery were good. The experimental results were compared with those obtained by use of solid-phase extraction and polymer monolithic microextraction. Because sample derivatization, extraction, and concentration were combined in a single step, the proposed method enabled simple, rapid, inexpensive, and efficient analysis of aldehydes in blood. The method has great potential for clinical analysis of biologically relevant aldehydes.

Keywords

Column liquid chromatography–tandem mass spectrometry Dispersive liquid–liquid microextraction Derivatization Aldehyde Human blood 
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Notes

Acknowledgments

The project was supported by the National Natural Science Foundation of China (no. 20805017), the China Postdoctoral Science Foundation (no. 20070420923), the Postdoctoral Science Special Foundation of China (no. 200801329), the Scientific and Technological Brainstorm Project of Wuhan (no. 200860423220), and the Open Foundation of Key Lab of Analytical Chemistry for Life Science, Ministry of Education, Nanjing University (no. KLACLS07002).

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Copyright information

© Vieweg+Teubner | GWV Fachverlage GmbH 2009

Authors and Affiliations

  1. 1.Department of ChemistryWuhan UniversityWuhanPeople’s Republic of China
  2. 2.Key Laboratory of Pesticide and Chemical Biology, College of ChemistryMinistry of Education, Central China Normal UniversityWuhanPeople’s Republic of China
  3. 3.Hubei Cancer HospitalWuhanPeople’s Republic of China

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