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Journal of Chromatography A
Volume 1160, Issues 1-2, 10 August 2007, Pages 114-119
23rd Montreux Symposium on Liquid Chromatography-Mass Spectrometry, Supercritical Fluid Chromatography-Mass Spectrometry, Capillary Electrophoresis-Mass Spectrometry and Tandem Mass Spectrometry, 23rd Montreux Symposium on Liquid Chromatography-Mass Spectrometry, Supercritical Fluid Chromatography-Mass Spectrometry, Capillary Electrophoresis-Mass Spectrometry and Tandem Mass Spectrometry
 
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doi:10.1016/j.chroma.2007.04.015    How to Cite or Link Using DOI (Opens New Window)
Copyright © 2007 Elsevier B.V. All rights reserved.

Polymer monolith microextraction with in situ derivatization and its application to high-performance liquid chromatography determination of hexanal and heptanal in plasma

Hui-Juan Zhanga, Jing-Fang Huanga, Bo Lina and Yu-Qi FengCorresponding Author Contact Information, a, E-mail The Corresponding Author

aDepartment of Chemistry, Wuhan University, Wuhan 430072, China

Received 18 January 2007; 
revised 1 April 2007; 
accepted 5 April 2007. 
Available online 19 April 2007.

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Abstract

A simple, rapid and sensitive method for the determination of hexanal and heptanal in plasma by high-performance liquid chromatography (HPLC) has been developed, which is based on polymer monolith microextraction (PMME) with in situ derivatization. 2,4-dinitrophenylhydrazine (DNPH) as a derivatizing reagent was first adsorbed on a poly (methacrylic acid-co-ethylene glycol dimethacrylate) (MAA-EGDMA) monolith, and then microextraction was performed simultaneously with derivatization on the monolith. The several parameters affecting the in situ derivatization simultaneously with PMME were investigated, including the flow rate, pH, buffer concentration, and temperature. The whole pretreatment process can be accomplished within 8 min. The limits of detection for hexanal and heptanal were found to be 2.4 and 3.6 nmol/L, respectively. The recoveries in plasma sample were in the range of 83–87% with the inter- and intra-day precisions less than 6.8%. This method was successfully applied to the analysis of hexanal and heptanal in plasma samples from different cancer patients.

Keywords: Polymer monolith microextraction; In situ derivatization; Hexanal; Heptanal; 2,4-dinitrophenylhydrazine (DNPH); HPLC

Article Outline

1. Introduction
2. Experimental
2.1. Chemicals and materials
2.2. Sample preparation
2.3. Apparatus and chromatographic conditions
2.4. In situ derivatization–PMME procedures
2.4.1. Mode 1: PMME simultaneously with in situ derivatization
2.4.2. Mode 2: PMME followed by in situ derivatization
3. Results and discussion
3.1. Comparison of two modes of PMME within situ derivatization
3.2. Factors affecting PMME with in situ derivatization
3.3. Analysis of hexanal and heptanal in plasma samples
4. Conclusion
Acknowledgements
References






Journal of Chromatography A
Volume 1160, Issues 1-2, 10 August 2007, Pages 114-119
23rd Montreux Symposium on Liquid Chromatography-Mass Spectrometry, Supercritical Fluid Chromatography-Mass Spectrometry, Capillary Electrophoresis-Mass Spectrometry and Tandem Mass Spectrometry, 23rd Montreux Symposium on Liquid Chromatography-Mass Spectrometry, Supercritical Fluid Chromatography-Mass Spectrometry, Capillary Electrophoresis-Mass Spectrometry and Tandem Mass Spectrometry
 
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