Teixidó E, Santos F J, Puignou L, Galceran M T
Departament de Química Analítica, Facultat de Química, Universitat de Barcelona, Martí i Franquès 1-11, 08028 Barcelona, Spain.
J Chromatogr A. 2006 Nov 24;1135(1):85-90. doi: 10.1016/j.chroma.2006.09.023. Epub 2006 Sep 28.
A new, simple and selective method for the analysis of 5-hydroxymethylfurfural (HMF) in foods by gas chromatography coupled to mass spectrometry (GC-MS) is proposed. Several derivatising procedures based on the formation of an HMF silylated derivative using different reagents were studied. Among the derivatising reagents examined, N,O-bis-trimethylsilyltrifluoroacetamide (BSTFA) provided the best derivatisation yield. Sample clean-up was also optimised, using either liquid-liquid extraction with dichloromethane or solid-phase extraction (SPE) with several commercially available cartridges, and the best results were obtained using ENV+ cartridges. Quality parameters such as day-to-day and run-to-run precision (RSD<10%), linearity (between 25 and 700 ng g(-1)) and detection limit (6 ng g(-1)) were established. This method was successfully applied to the analysis of HMF content in several Spanish food samples from a local market, such as jam, honey, orange juice and bakery products.
提出了一种通过气相色谱-质谱联用(GC-MS)分析食品中5-羟甲基糠醛(HMF)的新型、简单且选择性的方法。研究了几种基于使用不同试剂形成HMF硅烷化衍生物的衍生化程序。在所研究的衍生化试剂中,N,O-双(三甲基硅基)三氟乙酰胺(BSTFA)的衍生化产率最高。还对样品净化进行了优化,采用二氯甲烷液-液萃取或使用几种市售柱进行固相萃取(SPE),使用ENV+柱获得了最佳结果。确定了诸如日常和批次间精密度(RSD<10%)、线性(25至700 ng g(-1)之间)和检测限(6 ng g(-1))等质量参数。该方法成功应用于分析来自当地市场的几种西班牙食品样品中的HMF含量,如果酱、蜂蜜、橙汁和烘焙食品。