固相微萃取膜的研制及其在分析样品预处理中的应用-分析化学专业论文.docxVIP

萃取时间、解吸时间和解吸溶剂对萃取效率和解吸效率的影响。对PAl-ls的萃取 萃取时间、解吸时间和解吸溶剂对萃取效率和解吸效率的影响。对PAl-ls的萃取 分析，方法的线性范围在O．10～1000．00腭／L之间，检出限在O．01～O．32峪几之 间，RSD在5．4％～16．6％之间，分析实际江水样品，回收率在69．1％～100．2％ 之间，RSD在5．9％～24．7％之间。对酚类化合物的萃取分析，方法的线性范围 在O．10～5000．00雌／L之间，检出限在O．02～1．47 rtg／L之间，RSD在4．9％～13．1 ％之间，分析实际江水样品，回收率均在81．1％～105．4％之间，RSD在4．8％～ 16．3％之间。 4采用聚乙二醇二环氧甘油醚和13-cI)合成了新型的环糊精聚合物，并将 其作为涂层材料制各了聚乙二醇／B一环糊精(PEG／15-CD)固相微萃取膜。测试证 实膜的表面均匀一致，涂层材料耐溶剂、对基材的附着力好，同时研究了涂层材 料的热稳定性和热分解机理。采用自制PEG／p-CD固相微萃取膜，建立了SPMEM —Gc府喱s测定水样中PAHs和酚类化合物的分析方法，研究了萃取介质、萃取 时间、解吸时间和解吸溶剂对萃取效率和解吸效率的影响。对PAHs的萃取分析， 方法的线性范围在0．50～1000．00pg几之间，检出限在O．05～O．52雌／L之间，RSD 在4．0％～18．3％之间，分析实际江水样品，回收率在84．6％～116．3％之间，RSD 在4．3％～19．4％之间。对酚类化合物的萃取分析，方法的线性范围在0．10～ 1000．00峙／L之间，检出限在O．04～O．64岭几之间，RSD在6．3％～9．4％之间， 分析实际江水样品，回收率均在81．2％～91．4％之间，RSD在6．1％～11．3％之 间。 关键词：固相微萃取膜，溶胶一凝胶，多环芳烃，酚类化合物 Preparation Preparation of Sofid-Phase Mieroextraction Membrane and its Application in Sample Pre-treatment Major： Analytical Chemistry Name： Yang Yun-yun Supervisor：Prof．Li Gong-ke Solid-phase microextraction membrane(SPMEM)is a new sample pre-treatment technique，which combines sampling,extraction and concentration in one step． SPMEM inherns t11e extraction mechanism of SPME and has similar extraction performance as SPME．It is an important extension of SPME．In this thesis，three new SPMEM witll different polarity weft prepared and their applications in analysis of polycyclic aromatic hydrocarbons(PAHs)and phenols in water were studied．111e research contents are as follows： l皿e development,principle，characteristic，device，coating and application of SPME were reviewed．SPMEM was introduced，including its development，principle， application，advantage and shortcoming．Sol-gel technique and its application in SPME coating were also summarized． 2 A new polydimethysiloxane coated SPMEM was prepared．The coating was uniform and had good heat-stability,solvent-resistant ability and adhesion．A method for the determination of PAHs in water by SPMEM coupled with GC／MS was developed．111e exp