悬浮聚合法制备亲水-亲油型高分子固相萃取填料及其功能化研究  

Preparation of Hydrophilic-Lipophilic Composite Solid Phase Extraction Material by Suspension Polymerization and Its Functionalization

作　　者：包建民[1] 孙超慧[1] 李优鑫[1] 谢丹[1] 

机构地区：[1]天津大学药物科学与技术学院,天津市现代药物传递及功能高效化重点实验室,天津化学化工协同创新中心,天津300072

出　　处：《材料导报》2015年第20期1-7,共7页Materials Reports

基　　金：国家自然科学基金(21375093);高等学校博士学科点专项科研基金(20130032120081);天津大学自主创新基金(1102213)

摘　　要：采用悬浮聚合法合成了一种以二乙烯苯和N-乙烯吡咯烷酮为单体的高分子聚合物固相萃取填料（DVB-NVP）,系统地考察了引发剂、致孔剂、分散剂以及反应时间等对填料形态和粒径分布的影响,用光学显微镜对其进行表征,以农药作为模型化合物,结合紫外分光光度（UV）和高效液相色谱法（HPLC）对填料进行评价。同时对合成的微球进行官能团衍生,并优化衍生化条件。结果表明：以羟丙基甲基纤维素为分散剂,偶氮二异丁腈为引发剂时,于80℃下反应8h可制得粒径为20～60μm的单分散高交联亲水-亲油型聚合物,其对灭多威、福美林以及乙酰甲胺磷的回收率分别为97.34%、86.24%和96.96%,相对标准偏差分别为2.27%、0.96%、1.83%。4种衍生化DVB-NVP填料具有较高的离子交换容量。A hydrophilic-lipophilic balance solid phase extraction material was synthesized by suspension polymerization based on divinylbenzene and N-vinyl pyrrolidone（DVB-NVP）.Several factors including various initiators,porogens,dispersing agents and react time were investigated to further enhance the characteristics of packings.The morphosis of the microspheres was tested by electron microscope and its performance as a kind of solid phase extraction（SPE）resin was evaluated using pesticide residues combined with high-performance liquid chromatography（HPLC）and ultraviolet spectrophotometry（UV）.Then,the copolymer DVB-NVP was functionalized to modify the surface properties.The results indicated that the copolymer DVB-NVP with 20μm to 60μm could be obtained satisfactorily when the azobisisobutyronitrile was as the initiator,the HPMC was the dispersing agents,and the reaction time was 8hin 80°C.When real samples were pretreated by the prepared microspheres,the recovery for methomyl,thiram and acephate was 97.34%,86.24% and 96.96%,respectively,and the RSD% was 2.27%,0.96% and1.83%,respectively.For the four functionalized resins,their ion exchange capacities were able to similar,even be superior to commercial products.

关 键 词：亲水-亲油平衡 高分子聚合物 固相萃取 悬浮聚合法 功能化 

分 类 号：O63[理学—高分子化学]