应用化学
應用化學
응용화학
CHINESE JOURNAL OF APPLIED CHEMISTRY
2010年
2期
132-136
,共5页
李丽丽%周文辉%李永%林黎明%朱校斌%杨黄浩%王小如
李麗麗%週文輝%李永%林黎明%硃校斌%楊黃浩%王小如
리려려%주문휘%리영%림려명%주교빈%양황호%왕소여
软骨藻酸%分子印迹聚合物%记忆缺失性贝毒%固相萃取
軟骨藻痠%分子印跡聚閤物%記憶缺失性貝毒%固相萃取
연골조산%분자인적취합물%기억결실성패독%고상췌취
domoic acid%molecularly imprinted polymer%amnesia shellfish poisoning(ASP)%solid-phase extraction
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150 mg印迹聚合物填充于1.0 mL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2 mg/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).
以貝毒-軟骨藻痠的結構類似物1,3,5-戊烷三羧痠為模闆分子,4-乙烯基吡啶為功能單體,乙二醇二甲基雙丙烯痠酯為交聯劑,閤成瞭對軟骨藻痠具有較好選擇性的分子印跡聚閤物.經索氏提取去除模闆分子後,在聚閤物內部形成瞭與模闆分子1,3,5-戊烷三羧痠以及結構類似物軟骨藻痠呎吋、形狀以及活性基糰互補的結閤位點.通過靜態平衡結閤實驗研究瞭該聚閤物的結閤能力和選擇性能,與化學組成相同的相應非印跡聚閤物相比,1,3,5-戊烷三羧痠的分子印跡聚閤物對軟骨藻痠具有較高的吸附性能和選擇性.用150 mg印跡聚閤物填充于1.0 mL玻璃註射器製成的分子印跡固相萃取柱,採用離線模式,併結閤高效液相色譜實現紫貽貝和海水中軟骨藻痠的分離與檢測.對于加標2 mg/L的紫貽貝和海水樣品,迴收率分彆達到(93.4±4.9)%和(89.7±3.2)%(n=3).
이패독-연골조산적결구유사물1,3,5-무완삼최산위모판분자,4-을희기필정위공능단체,을이순이갑기쌍병희산지위교련제,합성료대연골조산구유교호선택성적분자인적취합물.경색씨제취거제모판분자후,재취합물내부형성료여모판분자1,3,5-무완삼최산이급결구유사물연골조산척촌、형상이급활성기단호보적결합위점.통과정태평형결합실험연구료해취합물적결합능력화선택성능,여화학조성상동적상응비인적취합물상비,1,3,5-무완삼최산적분자인적취합물대연골조산구유교고적흡부성능화선택성.용150 mg인적취합물전충우1.0 mL파리주사기제성적분자인적고상췌취주,채용리선모식,병결합고효액상색보실현자이패화해수중연골조산적분리여검측.대우가표2 mg/L적자이패화해수양품,회수솔분별체도(93.4±4.9)%화(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.