Beijing Key Laboratory for Microanalytical Methods and Instrumentation, Department of Chemistry, Tsinghua University, Beijing 100084, China.
Talanta. 2012 Jan 30;89:189-94. doi: 10.1016/j.talanta.2011.12.015. Epub 2011 Dec 9.
Hydrophilic carbon-functionalized magnetic microspheres coated with chitosan (Fe(3)O(4)@C@CHI) were synthesized for the first time. The hydrophilic carbonaceous layer on the Fe(3)O(4) microspheres was formed by the hydrothermal reaction of Fe(3)O(4) microspheres and glucose, and then chitosan was coated on surface of the carbon-functionalized microspheres by an easy zero-length reaction with 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC) and N-hydroxysuccinimide (NHS) as cross-linkers. The Fe(3)O(4)@C@CHI microspheres were spherical core-shell structure with uniform size at about 400 nm. The microspheres had a high saturation magnetization of 60.22 emu g(-1), which was sufficient for magnetic separation. The Fe(3)O(4)@C@CHI microspheres presented good hydrophilic property due to the abundant carboxyl and hydroxyl groups on the carbonaceous layer of the microspheres. The successful modification of chitosan on the surface of carbon-functionalized magnetic microspheres was validated by the adsorption of Eriochrome Black T (EBT). The prepared microspheres were applied as magnetic solid-phase extraction materials for extraction of bisphenol A (BPA) in aqueous samples. The extraction recoveries of spiked samples were in the range of 99.4-102.6% with low relative standard deviations of 2.8-3.9%. The results demonstrated that the novel Fe(3)O(4)@C@CHI microspheres were good candidate as magnetic SPE materials for extraction of analytes from aqueous samples.
首次合成了壳聚糖包覆的亲水碳功能化磁性微球(Fe(3)O(4)@C@CHI)。Fe(3)O(4)微球在葡萄糖的水热反应中形成亲水碳质层,然后通过 1-乙基-3-(3-二甲基氨基丙基)碳二亚胺(EDC)和 N-羟基琥珀酰亚胺(NHS)作为交联剂的简单零长度反应,在碳功能化微球表面涂覆壳聚糖。Fe(3)O(4)@C@CHI 微球呈球形核壳结构,粒径均匀,约为 400nm。微球具有 60.22 emu g(-1)的高饱和磁化强度,足以进行磁分离。由于微球碳质层上含有丰富的羧基和羟基,Fe(3)O(4)@C@CHI 微球具有良好的亲水性。通过对 Eriochrome Black T(EBT)的吸附验证了壳聚糖在碳功能化磁性微球表面的成功修饰。制备的微球用作磁性固相萃取材料,用于从水样中萃取双酚 A(BPA)。加标样品的萃取回收率在 99.4-102.6%范围内,相对标准偏差为 2.8-3.9%。结果表明,新型 Fe(3)O(4)@C@CHI 微球是从水样中萃取分析物的磁性 SPE 材料的良好候选材料。