2-4-dinitrophenylhydrazine and heptanal

In this study, magnetic solid phase extraction coupled with in-situ derivatization (MSPE-ISD) was established for the determination of hexanal and heptanal in human urine. 2,4-Dinitrophenylhydrazine (DNPH) was used as the derivatization reagent that was adsorbed onto the surface of magnetite/silica/poly(methacrylic acid-co-ethylene glycol dimethacrylate) (Fe3O4/SiO2/P(MAA-co-EGDMA)). And then simultaneous extraction and derivatization of the aldehydes were performed on the DNPH-adsorbed Fe3O4/SiO2/P(MAA-co-EGDMA). The simple, rapid and sensitive determination of hexanal and heptanal can be accomplished within 9min. Under optimized conditions, the limits of detection (LODs) were 1.7 and 2.5nmol/L for hexanal and heptanal, respectively. The relative recoveries ranged from 72.8% to 91.4% with the intra- and inter-day relative standard deviations (RSDs) being less than 9.6%. Furthermore, the proposed method was successfully applied to determine endogenous hexanal and heptanal in human urine from healthy persons and lung cancer patients. The results showed the higher concentrations of hexanal and heptanal were observed in lung cancer patients compared to healthy controls. Thus, the developed MSPE-ISD method is suitable for the determination of aldehydes in urines.

Topics: Aldehydes; Chromatography, High Pressure Liquid; Ferrosoferric Oxide; Humans; Lung Neoplasms; Magnetic Phenomena; Phenylhydrazines; Polymethacrylic Acids; Silicon Dioxide; Solid Phase Extraction

In this work, a polypropylene frit with porous network structure (20 μm pole size) was first utilized as the mould of polymer monolithic material, poly(methacrylic acid-co-ethylene glycol dimethacrylate) (MAA-co-EDMA) monolith was synthesized within channels and macropores of the frit. A simple and sensitive solid-phase microextraction method based on polymer monolith frit coupled with high-performance liquid chromatography (HPLC) was established and applied to analysis of hexanal and heptanal in biological samples (human urine and serum). In the method, small molecule metabolites (aldehydes) in biological samples derivatized with 2,4-dinitrophenylhydrazine (DNPH), and the formed hydrazones were extracted simultaneously on the monolithic frit and thereafter ultrasound-assisted desorbed with acetonitrile as elution solvent. The experimental parameters with regard to polymerization, derivatization and extraction were investigated. Under the optimal conditions, the linearity was in the range of 0.02-5.0 μmol L(-1) (r=0.9994) for both hexanal and heptanal and the limits of detection (S/N=3) were 0.81 nmol L(-1) for hexanal and 0.76 nmol L(-1) for heptanal. The relative standard deviations (RSDs, n=5) were less than 6.5% for the same monolithic frit and less than 8.9% for the different monolithic frits. Satisfactory recoveries ranging from 70.71% to 88.73% were obtained for the urine samples. The method possesses many advantages including simple setup, fast analysis, low cost, sufficient sensitivity, good biological compatibility and less organic solvent consumption. The proposed method is a useful assistant tool in the clinical early diagnosis of lung disease by monitoring aldehyde biomarker candidates in complex biological samples.

Topics: Aldehydes; Chromatography, High Pressure Liquid; Humans; Phenylhydrazines; Polypropylenes; Solid Phase Microextraction; Temperature

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.

Topics: Adult; Aldehydes; Chemistry Techniques, Analytical; Chromatography, High Pressure Liquid; Female; Humans; Hydrogen-Ion Concentration; Male; Middle Aged; Phenylhydrazines; Polymers; Temperature