基于磁性固相萃取的表面增强拉曼基底的制备及其在痕量环境污染物分析中的应用

Environmental pollutants, especially the persistent organic pollutants (POPs), have serious harm to the environment and human health due to its high toxicity, half volatile, persistent residual and biological accumulation. It’s highly urgent for the development of highly sensitive, convenient and rapid detection method. Environmental samples have the three features that cause the difficult to detect the POPs. The first, the POPs content was always very low. Second, the concentration of contents in sample had the huge variety. Last, there was very serious interference from matrix. So, the emphasis is to development the pretreatment method of high selectivity and high efficiency enrichment. In this project, the functional nanoparticles of Ag and magnetic particles are introduced to the ordered mesoporous carbon. It was as the magnetic solid adsorbent and modified by 4-nitrobenzene thiophenol for separation and enrichment of pollutants from the environment samples. Last, the analytical method was established by combining with the SERS spectra which has the high selectivity, quickness and abundant information of spectra. After the implement of the project, the magnetic material could be gained that had the ability of enrichment of trace pollutants; the analytical method could be established accurately and quickly. It’s very important meaning for monitoring environmental pollutants.

环境污染物特别是持久性有机污染物由于具有高毒性、半挥发性、长期残留性和生物蓄积性，对环境和人类健康具有严重危害，亟需高灵敏、方便、快速的检测方法。持久性污染物在环境样品中含量低，组分差异大，基质干扰严重，对检测造成了很大的困难，发展具有高选择性、高富集效率的前处理方法是核心所在。本项目拟将具有SERS特性的银纳米颗粒和具有磁分离特性的纳米颗粒引入有序介孔碳内，设计和制备银纳米颗粒嵌入的磁性有序介孔碳材料作为磁性固相吸附剂，利用4-硝基苯硫酚作为修饰剂对吸附剂进行结构修饰，实现对环境污染物的分离富集，最后结合表面增强拉曼光谱的高灵敏、快速、丰富的光谱信息实现对痕量环境污染物分析。本项目的实施，可以获得痕量污染物的磁性高效捕集材料，并建立痕量环境污染物准确、快速分析方法，对监控环境污染物具有十分重要的意义。

环境污染物特别是持久性有机污染物以及重金属污染，对环境和人类健康具有严重危害，亟需高灵敏、方便、快速的检测方法。持久性污染物在环境样品中含量低，组分差异大，基质干扰严重，对检测造成了很大的困难，发展具有高选择性、高富集效率的前处理方法是分析方法建立的核心所在。本项目一方面通过软模板法采用溶剂挥发自组装方式，以两性三嵌段共聚物F127为模板，可溶性低分子量的酚醛树脂预聚体为碳源，乙酰丙酮为偶合试剂，通过磁功能化，研制出银纳米颗粒负载磁性碳材料。第二个方面通过以油酸、氯化钙以及磷酸二氢钠为原料通过热熔法制备得到羟基磷灰石超长纳米线，然后，利用银离子与磷酸根的结合，制备得到银纳米颗粒负载的羟基磷灰石超长纳米线得到负载纳米银的内参比表面增强拉曼光谱试纸。利用这两种不同类型的表面增强拉曼光谱基底，分别建立了对痕量环境污染的快速高灵敏分析检测方法。同时，本项目还设计与制备磁功能化的稀土荧光材料，通过优化磁性固相萃取条件，建立和发展痕量环境污染物的高灵敏，快速检测分析方法。该项目的相关研究成果，已经在ACS Applied Materials and Interfaces、New Journal of Chemistry、Research on Chemical Intermediates、Analyst等学术期刊上发表标注本项目资助的论文6篇。申请中国发明专利4项，其中获得授权中国发明专利2项。培养本科生3名，硕士研究生1名，协助培养博士研究生2名。因此，本项目取得的成果已经完全达到项目考核或预定研究指标的要求。