School of Chemical Sciences, Universiti Sains Malaysia, 11800 Minden, Penang, Malaysia.
Talanta. 2010 Jan 15;80(3):1183-90. doi: 10.1016/j.talanta.2009.09.006.
Three sorbent materials (A18C6-MS, DA18C6-MS and AB18C6-MS) based on the crown ether ligands, 1-aza-18-crown-6, 1,4,10,13-tetraoxa-7,16-diazacyclo octadecane and 4'-aminobenzo-18-crown-6, respectively, were prepared by the chemical immobilization of the ligand onto mesoporous silica support. The sorbents were characterized by FT-IR, scanning electron microscopy-energy dispersive X-ray microanalysis, elemental analysis and nitrogen adsorption-desorption test. The applicability of the sorbents for the extraction of biogenic amines by the batch sorption method was extensively studied and evaluated as a function of pH, biogenic amines concentration, contact time and reusability. Under the optimized conditions, all the sorbents exhibited highest selectivity toward spermidine (SPD) compared to other biogenic amines (tryptamine, putrescine, histamine and tyramine). Among the sorbents, AB18C6-MS offer the highest capacity and best selectivity towards SPD in the presence of other biogenic amines. The AB18C6-MS sorbent can be repeatedly used three times as there was no significant degradation in the extraction of the biogenic amines (%E>85). The optimized procedure was successfully applied for the separation of SPD in food samples prior to the reversed-phase high performance liquid chromatography separation.
三种基于冠醚配体的吸附剂材料(A18C6-MS、DA18C6-MS 和 AB18C6-MS),分别为 1-氮杂-18-冠-6、1,4,10,13-四氧杂-7,16-二氮杂环十八烷和 4'-氨基苯并-18-冠-6,通过将配体化学固定在介孔硅载体上制备而成。采用傅里叶变换红外光谱(FT-IR)、扫描电子显微镜-能量色散 X 射线微分析(SEM-EDX)、元素分析和氮吸附-脱附测试对吸附剂进行了表征。作为 pH、生物胺浓度、接触时间和可重复使用性的函数,广泛研究和评估了吸附剂通过批量吸附法提取生物胺的适用性。在优化条件下,与其他生物胺(色胺、腐胺、组氨酸和酪胺)相比,所有吸附剂对亚精胺(SPD)表现出最高的选择性。在存在其他生物胺的情况下,AB18C6-MS 对 SPD 具有最高的容量和最佳选择性。AB18C6-MS 吸附剂可以重复使用三次,因为在提取生物胺时没有明显的降解(%E>85)。优化后的程序成功应用于食品样品中 SPD 的分离,然后进行反相高效液相色谱分离。