Department of Chemistry, Wuhan University, Wuhan 430072, PR China.
J Agric Food Chem. 2009 May 27;57(10):3981-8. doi: 10.1021/jf900434n. Epub 2009 Apr 27.
A simple and sensitive method for the determination of 5-hydroxymethylfurfural (HMF) in coffee, honey, beer, Coke, and urine by high-performance liquid chromatography (HPLC) is presented. This method is based on the formation of the 2,4-dinitrophenylhydrazone of HMF and subsequent polymer monolith microextraction (PMME) of this derivative. A poly(methacrylic acid-co-ethylene glycol dimethacrylate) (MAA-co-EGDMA) monolithic capillary column was selected as the extraction medium. Several parameters affecting the derivatization of HMF with 2,4-dinitrophenylhydrazine (DNPH) followed by extraction of the derivative were optimized. The procedure is simple and offers high sensitivity and specificity since the derivative of HMF is well preconcentrated by PMME with poly(MAA-co-EGDMA) monolith and well separated from the other components of the samples under examination. The recoveries in coffee, honey, beer, Coke, and urine samples were in the range of 83.9-110.8% spiked at different levels with HMF. The inter- and intraday precisions were less than 10%. The LOD (S/N = 3) and LOQ (S/N = 10) for HMF were 1.0 ng/mL and 3.4 ng/mL, respectively.
一种用于通过高效液相色谱法（HPLC）测定咖啡、蜂蜜、啤酒、可乐和尿液中 5-羟甲基糠醛（HMF）的简单灵敏的方法。该方法基于 HMF 与 2,4-二硝基苯肼（DNPH）形成腙，随后对该衍生物进行聚合物整体微萃取（PMME）。选择聚（甲基丙烯酸-co-乙二醇二甲基丙烯酸酯）（MAA-co-EGDMA）整体毛细管柱作为萃取介质。优化了影响 HMF 与 2,4-二硝基苯肼（DNPH）衍生化，然后萃取衍生物的几个参数。该方法简单，具有高灵敏度和特异性，因为 HMF 的衍生物通过 PMME 与聚（MAA-co-EGDMA）整体很好地预浓缩，并与被检测样品的其他成分很好地分离。在咖啡、蜂蜜、啤酒、可乐和尿液样品中，HMF 的回收率在不同水平下为 83.9-110.8%。日内和日间精密度均小于 10%。HMF 的检出限（S/N = 3）和定量限（S/N = 10）分别为 1.0 ng/mL 和 3.4 ng/mL。
