两种新型固相微萃取纤维的研制和表征  

Preparation and characterization of two new fibers for solid phase microextraction

作　　者：杨红丽[1] 王镨[2] 王翊如[3] 朱四喜[4] 

机构地区：[1]浙江海洋学院食品与药学学院,浙江舟山316000 [2]浙江大学出版社,浙江杭州310028 [3]厦门大学现代分析科学教育部重点实验室,福建厦门361005 [4]浙江海洋学院海洋科学学院,浙江舟山316000

出　　处：《浙江大学学报（工学版）》2008年第7期1276-1280,共5页Journal of Zhejiang University：Engineering Science

基　　金：国家"863"高技术研究发展计划资助项目(2002AA639390);浙江省自然科学基金资助项目(Y506231)

摘　　要：采用十八烷基键合硅胶(C18)和碳纳米管(CNTs)制备了多孔的C18固相微萃取(SPME)纤维和碳纳米管(CNTS)固相微萃取纤维,扫描电镜结果显示两种纤维表面均细致紧密.应用固相微萃取气相色谱离子阱质谱(SPME-GC-MS)联用技术分析邻苯二甲酸酯(PEs),对两种纤维的性能进行表征.结果显示,两种自制纤维均具有和商品纤维聚二甲基硅氧烷(PDMS)、聚乙二醇(PA)相当的吸附特性和重现性,多孔C18纤维因C18键合硅胶的吸附表面积大、活性膜薄,萃取速率快,萃取效率高,在本实验条件下,萃取邻苯二甲酸甲酯(DMP)和邻苯二甲酸乙酯(DEP)30 min可以达到平衡状态;对邻苯二甲酸酯类中等极性的化合物的富集倍数在103以上.碳纳米管纤维具有巨大的表面积和较强的吸附性能,萃取容量与商品涂层不相上下,但其达到平衡的时间比C18纤维稍长.Two porous solid phase microextraction （SPME） fibers were made by C18 bonded silica （C18） and carbon nanotubes （CNTs） . The analysis results by electron micrographs indicate that the fiber surface is clinged uniformly and closely. The analytical performances of the two fibers were evaluated by solid-phase microextraction coupling gas chromatography ion trap detector determining phthalate esters （PEs）. The two fibers have the same good adsorption properties and precision as the commercial polydimethylsiloxane （PDMS） and polyacrylate （PA） fibers. The mass transfer rate of the analysts is very fast from the sample solution to the fiber when coated with C18 stationary for the large adsorption area and thin coat of C18. It can reach equilibrium in 30 min to both dimethyl phthalate （DMP） and diethyl phthalate （DEP）. The concentration factor of middling polarity phthalate esters between C18 stationary phase and sample solution is above 10^3. The fiber coated commercial fibers. But they CNTs have larger adsorption area and ability, and their capacity are as good as take longer time to reach equilibrium than fiber coated C18.

关 键 词：碳纳米管 C18键合硅胶 固相微萃取 

分 类 号：O657[理学—分析化学] TQ028[理学—化学]