软骨藻酸分子印迹聚合物的制备及其固相萃取应用  

Synthesis of Domoic Acid Imprinted Polymer and Its Extraction Application

作　　者：李丽丽[1] 周文辉[2,3] 李永[2] 林黎明[4] 朱校斌[1] 杨黄浩[3] 王小如[2,3] 

机构地区：[1]中国科学院海洋研究所 [2]中国海洋大学化学化工学院 [3]国家海洋局第一海洋研究所,青岛266061 [4]山东出入境检验检疫局技术中心

出　　处：《应用化学》2010年第2期132-136,共5页Chinese Journal of Applied Chemistry

基　　金：国家自然科学基金(20775019);国家"八六三"计划(2006AA09Z168);山东省自然科学基金(Y2006B01);青岛市自然科学基金(08-1-3-32-JCH);国家海洋局青年基金(2007601)资助项目

摘　　要：以贝毒-软骨藻酸的结构类似物1,3,5-戊烷三羧酸为模板分子,4-乙烯基吡啶为功能单体,乙二醇二甲基双丙烯酸酯为交联剂,合成了对软骨藻酸具有较好选择性的分子印迹聚合物。经索氏提取去除模板分子后,在聚合物内部形成了与模板分子1,3,5-戊烷三羧酸以及结构类似物软骨藻酸尺寸、形状以及活性基团互补的结合位点。通过静态平衡结合实验研究了该聚合物的结合能力和选择性能,与化学组成相同的相应非印迹聚合物相比,1,3,5-戊烷三羧酸的分子印迹聚合物对软骨藻酸具有较高的吸附性能和选择性。用150mg印迹聚合物填充于1.0mL玻璃注射器制成的分子印迹固相萃取柱,采用离线模式,并结合高效液相色谱实现紫贻贝和海水中软骨藻酸的分离与检测。对于加标2mg/L的紫贻贝和海水样品,回收率分别达到(93.4±4.9)%和(89.7±3.2)%(n=3)。Domoic acid （DA） was used as the target compound, its structural analog 1,3,5-pentanetri- carboxylic acid was used as template molecules, 4-vinyl pyridine as the functional monomer and ethylene glycol dimethacrylate as the cross-linking agent for the preparation of the molecularly imprinted polymers （MIPs）. After Soxhlet extraction of the template 1,3,5-pentanetricarboxylic acid, binding sites were formed in the polymer with complementary size, shape, and positioning of chemical functionalities to 1,3,5- pentanetricarboxylic acid and also structural analog domoic acid. The molecularly imprinted polymer was investigated with the aid of equilibrium binding experiments to evaluate the molecular recognition and binding characteristics of the imprinted polymer. The results show that compared with non-imprinted polymer, the imprinted polymer exhibits a much higher affinity for domoic acid. The molecularly imprinted solid-phase extraction（MISPE） columns were prepared from a 1.0 mL glass syringe packed with 150 mg of the molecularly polymer. The MISPE procedure performed in an off-line mode coupled with reversed-phase high performance liquid chromatography was developed to extract domoic acid from Mytilus edulis and seawater samples. The mean recoveries of domoic acid from Mytilus edulis and artificial seawater spiked with 2 mg/L domoic acid were （93.4±4.9 ） % and （ 89.7 ±3.2 ） % （ n = 3 ）, respectively.

关 键 词：软骨藻酸 分子印迹聚合物 记忆缺失性贝毒 固相萃取 

分 类 号：O658[理学—分析化学]