Development of a novel monolith frit-based solid-phase microextraction method for determination of hexanal and heptanal in human serum samples

• Published in: Journal of separation science Vol. 35; no. 5-6; pp. 713 - 720
• Main Authors: Xu, Hui, Yan, Zhihua, Song, Dandan
• Format: Journal Article
• Language: English
• Published: Weinheim Blackwell Publishing Ltd 01.03.2012; Wiley
• Subjects: Adsorption; Aldehydes; Aldehydes - blood; Aldehydes - isolation & purification; Aldehydes / Monolith frit / High-performance liquid chromatography / Serum analysis / Solid-phase microextraction; Biological and medical sciences; Chromatography, High Pressure Liquid; Columnar structure; Frit; Human; Humans; Hydrazones; Investigative techniques, diagnostic techniques (general aspects); Liquid chromatography; Medical sciences; Miscellaneous. Technology; Pathology. Cytology. Biochemistry. Spectrometry. Miscellaneous investigative techniques; Polymerization; Polypropylenes - chemistry; Serums; Solid Phase Microextraction - instrumentation; Solid Phase Microextraction - methods; Biological fluid; Chemical analysis; Lung cancer; HPLC chromatography; Solid-phase microextraction; Derivatization; Aldehydes; Blood; Chemical enrichment; Surface structure; Characterization; Crosslinked copolymer; Methacrylic acid copolymer; Sample preparation; Clinical biology; Bronchus disease; Serum analysis; Adsorbent; Quantitative analysis; Photochemical copolymerization; Trace analysis; Human; Lung disease; Scanning electron microscopy; Healthy subject; Respiratory disease; Aliphatic compound; Propylene polymer; Monolithic column; Monolith frit; Patient; Malignant tumor; Aldehyde; High-performance liquid chromatography; Solid phase microextraction; Ultraviolet detector; Morphology; Preparation; Blood serum; Cancer
• ISSN: 1615-9306; 1615-9314; 1615-9314
• DOI: 10.1002/jssc.201100908

In this paper, a polypropylene frit with porous network structure and high area‐to‐thickness ratio (4.8 mm diameter, 1.6 mm thickness, 20 mm pore size) was utilized as a mould of monolith. Poly(methacrylic acid‐ethlyene glycol dimethacrylate) (MAA‐EGDMA) monolith was in situ synthesized in the micro‐channel of frit by photopolymerization. A monolith frit‐based solid‐phase microextraction method (SPME) was developed for the determination of hexanal and heptanal in serum samples by combining with high‐performance liquid chromatography. 2,4‐Dinitrophenylhydrazine (DNPH) as the derivatizing reagent was absorbed on a monolith frit, then its derivatization reaction with aldehydes and the absorption of formed hydrazones on the monolith disk occurred simultaneously. The condition parameters for polymerization, derivatization and extraction were optimized systematically. Under the optimum conditions, rigid structure, low back‐pressure and high column capacity were achieved for the monolith frit. The limits of detection for hexanal and heptanal were 1.86 and 1.38 nmol/L, respectively. The inter‐ and intra‐day relative standard deviations were less than 7.7% (n = 6). This method was applied successfully to aldehydes analysis in human serum samples. The method possesses advantages such as simplicity, efficiency, low cost and good biocompatibility. It provides an alternative approach for quantification of aldehydes in complex biological samples.