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Gas chromatography-mass spectrometric analysis of hexanal and heptanal in human blood by headspace single-drop microextraction with droplet derivatization
Authors:Li Ning  Deng Chunhui  Yin Xinying  Yao Ning  Shen Xizhong  Zhang Xiangmin
Affiliation:Department of Chemistry, Fudan University, Shanghai 200433, China.
Abstract:
In this work, we developed a new approach to the analysis of the lung cancer biomarkers, hexanal and heptanal in human blood that was based on headspace single-drop microextraction (HS-SDME) with droplet derivatization, followed by gas chromatography-mass spectrometry (GC-MS). Aldehydes in blood were headspace extracted, concentrated, and derivatized by a suspended microdrop solvent containing the derivatization agent O-(2,3,4,5,6-pentafluorobenzyl)hydroxylamine hydrochloride. The aldehyde oximes formed in the microdrop solvent were analyzed by GC-MS. The optimal HS-SDME with droplet derivatization parameters extraction solvent of decane, sample temperature of 40 degrees C, extraction time of 6 min, stirring rate of 1100 rpm, and solvent volume of 2.0 microL were obtained and used for analysis of hexanal and heptanal in blood. The method reproducibility, linearity, recovery, and detection limit were studied and the obtained results demonstrated the method feasibility. Finally, the proposed method was applied to the quantification of hexanal and heptanal in cancer blood and normal blood. Due to sample extraction, concentration, and derivatization being performed in a single step, the method provided a simple, rapid, low-cost, and efficient approach to analysis of aldehydes in blood samples.
Keywords:Hexanal   Heptanal   Headspace single-drop microextraction   Droplet derivatization   Blood analysis   Biomarker
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