Key Laboratory of Pesticide & Chemical Biology, Ministry of Education, College of Chemistry, Central China Normal University, Wuhan, PR China.
J Sep Sci. 2012 Mar;35(5-6):713-20. doi: 10.1002/jssc.201100908. Epub 2012 Jan 24.
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.
本文利用具有多孔网络结构和高纵横比（4.8 毫米直径，1.6 毫米厚度，20 毫米孔径）的聚丙烯 frit 作为整体的模具。通过光聚合，在 frit 的微通道中原位合成聚（甲基丙烯酸-乙二醇二甲基丙烯酸酯）（MAA-EGDMA）整体柱。结合高效液相色谱法，提出了一种基于整体柱 frit 的固相微萃取方法（SPME），用于血清样品中己醛和庚醛的测定。2,4-二硝基苯肼（DNPH）作为衍生化试剂被吸收到整体柱 frit 上，然后与醛发生衍生化反应，同时形成的腙被吸收到整体柱盘上。系统优化了聚合、衍生化和萃取的条件参数。在最佳条件下，得到了刚性结构、低背压和高柱容量的整体柱 frit。己醛和庚醛的检测限分别为 1.86 和 1.38 nmol/L。日内和日间相对标准偏差均小于 7.7%（n = 6）。该方法成功地应用于人血清样品中醛的分析。该方法具有简单、高效、低成本和良好的生物相容性等优点，为复杂生物样品中醛的定量分析提供了一种替代方法。
