基于聚甲基丙烯酸酯多孔材料的表面增强拉曼光谱检测方法研究
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摘要
作为一种快速灵敏的分析技术,表面增强拉曼散射(surface-enhanced Raman scattering, SERS)在痕量物质检测中得到越来越多的关注。本论文基于聚甲基丙烯酸缩水甘油酯-乙二醇二甲基丙烯酸酯(GMA-EDMA)多孔材料,结合银纳米颗粒发展出不同形式的增强基底,用于痕量物质的超灵敏表面增强拉曼检测。
以柱状的GMA-EDMA多孔材料为基底,成功建立了超灵敏的SERS检测方法。多孔材料表面形态能够提供变化的空隙和孔洞,有利于银纳米颗粒间产生“热点”,促进增强作用的发生。这种方法的灵敏度极高,可以得到浓度低至10-18mol/L的罗丹明6G(R6G)及10-16mol/L的对巯基苯胺(PATP)的SERS信号。此外,利用该基底成功实现了低含量的生物样品及农药的SERS检测,为今后将多孔材料上的超灵敏表面增强拉曼技术推广到现场检测奠定基础。
在前面工作的基础上,将柱状多孔材料改为粉末状,并设计了一套装置适合于微量样品快速检测。此方法在保留了以GMA-EDMA多孔材料为基底的超灵敏度的同时大大缩短了检测所需时间,相应的被测样品量也大大减少。利用该方法同样可以检测到10-18mol/L R6G的信号,并且提高了检测精密度。同时也成功实现了四种农药噻菌灵、三环唑、百草枯和敌草快的低浓度快速检测,能检测到的最低浓度分别为0.27mg/L,5×10-3mg/L,0.05mg/L和1×10-3mg/L。这项快速灵敏的检测方法具有推广到实际样品的检测中的意义。
金属溶胶虽然具有良好增强性能,但容易发生聚集使得纳米颗粒间的间距无法控制,难于给出重复性好的结果。为了进一步合成均匀性更好的增强基底,利用GMA-EDMA材料的结构特点,进行氨基改性后将银纳米颗粒自组装到材料表面,控制纳米颗粒的间距,提高结果重复性,制备出均一性更好的增强基底。发展的粉末状银自组装GMA-EDMA多孔材料基底具有增强性能优良,体积小巧,成本低廉,重复性好的优点。此基底能够避免大部分疏水性农药与溶胶混合的困难,也减少了实验步骤(只需将被测样品直接加在基底上即可采集SERS光谱),非常适合于SERS现场检测。成功检测了低浓度下的乐果和多菌灵,能检测到的最低浓度分别为0.1mg/L和0.625mg/L。与前面方法相比,结果重复性显著提高。所用的增强基底在适当保存条件下能够保存一个月,是一种相对稳定的增强基底,配合便携式拉曼光谱,其优良的性能将在现场低浓度物质检测中发挥巨大的作用。
As a sensitive analytical technique, surface-enhanced Raman scattering (SERS) has attracted more and more concern in trace detection. Based on poly(glycidyl methacrylate-ethylene dimethacrylate (GMA-EDMA) porous material combining with silver nanoparticles, several kinds of enhancement substrates were developed for ultrasensitive SERS detection.
A novel ultrasensitive SERS detection method was established based on the GMA-EDMA porous material in rod shape. The topography of this porous material could supply gaps and/or pores which were beneficial for the generation of "hot spots" that were essential to enhancement effect. This method was so sensitive that SERS signals of probe molecules of Rhodamine6G (R6G) and p-aminothiophenol (PATP) at concentrations as low as10-18mol/L and10"16mol/L could be detected. Biology samples and pesticides were successfully detected by this method. The ultrasensitive SERS based on porous material method showed promising features in on-site detection.
An investigation of rapid SERS detection method was developed by using porous material in powder shape, the shape of porous material was changed from rod to powder. Meanwhile, a set of device was developed by using this powder-shape porous material, which fitted the rapid detection of micro-sample volume. The feature of ultrasensitivity was retained, furthermore, the detection time and the required sample volume were also significantly reduced with this device. By this method, R6G at concentration of10"18mol/L was detected. Meanwhile, the precision of the method was improved. Four pesticides (thiabendazole, tricyclazole, paraquat and diquat) were also detected at the concentrations of0.27mg/L,5×10-3mg/L,0.05mg/L and1×10-3mg/L. This rapid and sensitive detection method was meaningful in practical sample detection.
Although metal colloid showed good performances in SERS enhancement, the aggragation of this kind of colloid led to uncontrollable distances between nanoparticles which result in poor signal-reproducibility. In order to achieve a uniform substrate, the GMA-EDMA porous material was modified with ammonia. With this modification, the silver nanoparticles could self-assemble onto the porous material surface. With this procedure, a uniform substrate was attained, and correspondingly the signal-reproducibility was improved. The Ag-self-assemble GMA-EDMA porous material in powder shape showed advantages like good enhancement performances, miniaturization, low price and good reproducibility. By this substrate, the mixing of colloid and hydrophobic pesticides could be avoided, which was normally difficult in operation. The procedure of the experiment was simplified (SERS spectrum could be collected after the addition of sample onto the substrate). This made the substrate suitable in on-site SERS detection. Dimethoate and carbendazim at concentrations of0.1mg/L and0.625mg/L were detected using this substrate, and the reproducibility was improved dramatically. With a portable storeage, the substrate showed a long-term stability for one month. Combining with a portable Raman instrument, excellent performances of this substrate have shown attractive potential in on-site detection of low concentration samples.
以柱状的GMA-EDMA多孔材料为基底,成功建立了超灵敏的SERS检测方法。多孔材料表面形态能够提供变化的空隙和孔洞,有利于银纳米颗粒间产生“热点”,促进增强作用的发生。这种方法的灵敏度极高,可以得到浓度低至10-18mol/L的罗丹明6G(R6G)及10-16mol/L的对巯基苯胺(PATP)的SERS信号。此外,利用该基底成功实现了低含量的生物样品及农药的SERS检测,为今后将多孔材料上的超灵敏表面增强拉曼技术推广到现场检测奠定基础。
在前面工作的基础上,将柱状多孔材料改为粉末状,并设计了一套装置适合于微量样品快速检测。此方法在保留了以GMA-EDMA多孔材料为基底的超灵敏度的同时大大缩短了检测所需时间,相应的被测样品量也大大减少。利用该方法同样可以检测到10-18mol/L R6G的信号,并且提高了检测精密度。同时也成功实现了四种农药噻菌灵、三环唑、百草枯和敌草快的低浓度快速检测,能检测到的最低浓度分别为0.27mg/L,5×10-3mg/L,0.05mg/L和1×10-3mg/L。这项快速灵敏的检测方法具有推广到实际样品的检测中的意义。
金属溶胶虽然具有良好增强性能,但容易发生聚集使得纳米颗粒间的间距无法控制,难于给出重复性好的结果。为了进一步合成均匀性更好的增强基底,利用GMA-EDMA材料的结构特点,进行氨基改性后将银纳米颗粒自组装到材料表面,控制纳米颗粒的间距,提高结果重复性,制备出均一性更好的增强基底。发展的粉末状银自组装GMA-EDMA多孔材料基底具有增强性能优良,体积小巧,成本低廉,重复性好的优点。此基底能够避免大部分疏水性农药与溶胶混合的困难,也减少了实验步骤(只需将被测样品直接加在基底上即可采集SERS光谱),非常适合于SERS现场检测。成功检测了低浓度下的乐果和多菌灵,能检测到的最低浓度分别为0.1mg/L和0.625mg/L。与前面方法相比,结果重复性显著提高。所用的增强基底在适当保存条件下能够保存一个月,是一种相对稳定的增强基底,配合便携式拉曼光谱,其优良的性能将在现场低浓度物质检测中发挥巨大的作用。
As a sensitive analytical technique, surface-enhanced Raman scattering (SERS) has attracted more and more concern in trace detection. Based on poly(glycidyl methacrylate-ethylene dimethacrylate (GMA-EDMA) porous material combining with silver nanoparticles, several kinds of enhancement substrates were developed for ultrasensitive SERS detection.
A novel ultrasensitive SERS detection method was established based on the GMA-EDMA porous material in rod shape. The topography of this porous material could supply gaps and/or pores which were beneficial for the generation of "hot spots" that were essential to enhancement effect. This method was so sensitive that SERS signals of probe molecules of Rhodamine6G (R6G) and p-aminothiophenol (PATP) at concentrations as low as10-18mol/L and10"16mol/L could be detected. Biology samples and pesticides were successfully detected by this method. The ultrasensitive SERS based on porous material method showed promising features in on-site detection.
An investigation of rapid SERS detection method was developed by using porous material in powder shape, the shape of porous material was changed from rod to powder. Meanwhile, a set of device was developed by using this powder-shape porous material, which fitted the rapid detection of micro-sample volume. The feature of ultrasensitivity was retained, furthermore, the detection time and the required sample volume were also significantly reduced with this device. By this method, R6G at concentration of10"18mol/L was detected. Meanwhile, the precision of the method was improved. Four pesticides (thiabendazole, tricyclazole, paraquat and diquat) were also detected at the concentrations of0.27mg/L,5×10-3mg/L,0.05mg/L and1×10-3mg/L. This rapid and sensitive detection method was meaningful in practical sample detection.
Although metal colloid showed good performances in SERS enhancement, the aggragation of this kind of colloid led to uncontrollable distances between nanoparticles which result in poor signal-reproducibility. In order to achieve a uniform substrate, the GMA-EDMA porous material was modified with ammonia. With this modification, the silver nanoparticles could self-assemble onto the porous material surface. With this procedure, a uniform substrate was attained, and correspondingly the signal-reproducibility was improved. The Ag-self-assemble GMA-EDMA porous material in powder shape showed advantages like good enhancement performances, miniaturization, low price and good reproducibility. By this substrate, the mixing of colloid and hydrophobic pesticides could be avoided, which was normally difficult in operation. The procedure of the experiment was simplified (SERS spectrum could be collected after the addition of sample onto the substrate). This made the substrate suitable in on-site SERS detection. Dimethoate and carbendazim at concentrations of0.1mg/L and0.625mg/L were detected using this substrate, and the reproducibility was improved dramatically. With a portable storeage, the substrate showed a long-term stability for one month. Combining with a portable Raman instrument, excellent performances of this substrate have shown attractive potential in on-site detection of low concentration samples.
引文
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