甲基膦酸■哪酯分子印迹聚合物的合成与识别特性研究  

Study on Synthesis of O-Pinacolyl Methylphosphonic Acid-imprinted Polymer Microspheres and Their Recognition Characteristics

作　　者：李盛菘 郑永超 钟近艺 赵冲林 LI Sheng-song;ZHENG Yong-chao;ZHONG Jin-yi;ZHAO Chong-lin(Research Institute of Chemical Defense,Academy of Military Sciences,Beijing102205,China;State Key Laboratory of NBC Protection for Civilian,Beijing102205,China)

机构地区：[1]中国人民解放军军事科学院防化研究院,北京102205 [2]国民核生化灾害防护国家重点实验室,北京102205

出　　处：《分析测试学报》2019年第7期775-783,共9页Journal of Instrumental Analysis

摘　　要：利用31P{1H}NMR谱和1HNMR谱、FT-IR谱等技术手段,研究了化学毒剂梭曼的降解产物(甲基膦酸[口频]哪酯)与甲基丙烯酸、丙烯酰胺功能单体的分子间作用力。通过预组装体系设计,合成了多孔性材料甲基膦酸[口频]哪酯分子印迹聚合物。通过Scatchard模型分析,得到该聚合物对甲基膦酸[口频]哪酯的最大表观结合量Qmax为661μg/g(AM为单体),在低吸附量(Q<500μg/g)范围内,吸附量对模板浓度的比值与吸附量呈线性相关。通过静态吸附分配实验发现,该聚合物对同系的5种烷基膦酸单烷基酯存在选择性,对结构不同的其他化合物的识别因子显著降低。将该分子印迹聚合物制成固相萃取柱,用于含大量背景干扰的样品中痕量甲基膦酸[口频]哪酯的萃取分离,取得显著效果。该研究为复杂基质中该类化合物的痕量分析鉴定提供了技术手段。The porous material O-pinacolyl methylphosphonic acid-imprinted polymer microspheres were synthesized through designing pre-assembly system,based on the interaction between the degradation product of Soman(O-pinacolyl methylphosphonic acid) molecules with methylacrylic acid and acrylamide functional monomer molecules discussed by techniques such as 31 P { 1H}NMR spectroscopy and 1H NMR spectroscopy.Scatchard analysis showed that the maximum apparent binding amount Q max was 661 μg/g(AM as monomer),and a straight line was presented in the diagram of a low adsorption range( Q <500 μg/g).In static adsorption experiment,the polymer was observed to be regularly selective to homologous five alkyl phosphonates monoalkyl esters,and the identification factors α to other compounds with different structures were decreased obviously.A solid phase extraction column using this synthesized polymer microsheres was used in the separation of trace O-pinacolyl methylphosphonic acid containing a large number of interferents with a remarkable effect.Results showed that the polymer synthesized provided an effective means for analysis and identification of trace degradation products of related chemical warfare agents in the complex samples.

关 键 词：化学毒剂 甲基膦酸[口频]哪酯 分子印迹聚合 痕量分析 固相萃取 

分 类 号：O657[理学—分析化学]