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.
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)
出处
《分析测试学报》
CAS
CSCD
北大核心
2019年第7期775-783,共9页
Journal of Instrumental Analysis
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
chemical warfare agents
O-pinacolyl methylphosphonic acid
molecule imprinted polymer
trace analysis
solid phase extraction
