应用介孔碳作为固相微萃取纤维涂层材料萃取挥发性芳香化合物
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摘要
固相微萃取技术(SPME),是一种新型的样品预处理技术,集采样、萃取、进样于一体,并可与多种分析仪器相结合,实现对目标物的快速分析与测定。碳材料一直被作为萃取有机化合物的吸附剂。介孔碳材料是一种新型的先进碳材料,其独特的结构和性能,如高的比表面积、好的热稳定性和耐化学性、大的孔体积和多样化的结构,使得介孔碳在吸附~([1])、催化~([2])和电化学~([3])方面具有吸引力。本实验以MCM-41为模板,蔗糖作为碳源,制备出新的介孔碳(C-MCM-41),通过溶胶-凝胶技术,将C-MCM-41作为涂层材料制备SPME纤维。将自制SPME纤维与GC-MS相结合建立了挥发性芳香化合物分析方法,并成功应用于萃取测定茶饮品中的5种VACs。五种VACs的线性范围为0.1~15.0μg/L,相关系数(r)为0.9923~0.9982,检出限(LODs)为5.0~10.0 ng/L,茶样品在1.0 ng/L和10.0 ng/L两个浓度水平上VACs的加标回收率在73.1%到99.1%之间。
In this work,a mesoporous carbon was fabricated using MCM-41 as a template and sucrose as a carbon source.The carbon material was coated on stainless-steel wires by using the sol-gel technique.The prepared solid-phase microextraction fiber was used for the extraction of five volatile aromatic compounds(chlorobenzene,ethylbenzene,o-xylene,bromobenzene,and 4-chlorotoluene) from tea beverage samples(red tea and green tea)prior to gas chromatog- raphy with mass spectrometric detection.The linearity was observed in the range from 0.1to 10.0 μg/L with the correlation coefficients(r) ranging from 0.9923 to 0.9982 and the limits of detection were less than 10.0 ng/L.The recoveries of the volatile aromatic compounds by the method from tea beverage samples at spiking levels of 1.0 and 10.0 μg/L ranged from 73.1 to 99.1%.
引文
[1]Hu X.;Pan J.;Hu Y.Preparation and evaluation of solid-phase microextraction fiber based on molecularly imprinted polymers for trace analysis of tetracyclines in complicated samples.Journal of Chromatography A,2008.1188(2):97-107.
    [2]Wang C.;Ma R.;Wu Q.;Wang Z.Magnetic porous carbon as an adsorbent for the enrichment of chlorophenols from water and peach juice samples.Journal of Chromatography A,2014.1361:60-66.
    [3]Su F.;Zeng J.;Bao X.Preparation and characterization of highly ordered graphitic mesoporous carbon as a Pt catalyst support for direct methanol fuel cells.Chemistry of materials,2005.17(15):3960-3967.

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