反相气相色谱研究分子印迹聚合物的气相识别
发布时间：2019-03-30 17:07
【摘要】：本论文分别以甲苯、糠酸、丹皮酚及桃金娘烯醛为目标分子,选取不同聚合方法制得分子印迹聚合物,利用不同表征方式测试其结构,并将其作为气相色谱固定相,采用反相气相色谱技术开展了一些其对气态模板分子的保留吸附研究。探究了固定相对气态目标分子的选择作用及键合能力,测得了目标分子在印迹柱上的吸附等温线,并测试了分子印迹聚合物对分析样品中模板的实际吸附作用,具体摘要如下:(1)以甲苯为致孔剂(又作为模板分子)结合沉淀聚合法,以四乙烯基吡啶为功能单体制备了甲苯印迹聚合物均匀微球。采用氮吸附法及光学显微镜测定了微球的结构特征,利用反相气相色谱法研究了其对气态甲苯分子及相关化合物的选择保留能力,探讨了印迹材料及对照聚合物对模板的等温键合能力。结果表明:甲苯印迹(MIP3)气相色谱柱对气态甲苯分子具有较高的选择保留能力,在优化色谱条件下,其对甲苯的保留因子和印迹因子分别高达68.42和7.049,对甲苯的选择因子相对于苯和对二甲苯分别为4.821和5.370,且能有效分离甲苯、苯及对二甲苯的模拟混合物(甲苯与对二甲苯及苯的分辨率分别为5.138和1.762)。甲苯印迹微球对气态甲苯的吸附等温线类型表现为BET吸附的Ⅱ类吸附。所得甲苯印迹材料对室内空气中的甲苯、苯及对二甲苯均具有较高的脱除能力。(2)以糠酸为模板分子制备了糠酸印迹聚合物,利用红外光谱和扫描电镜测定其结构特征。将其作为气相色谱固定相,采用反相气相色谱法对印迹柱的保留选择性能进行研究,测试了其对目标分子及结构类似物的键合能力,探究了其对样品模拟液中糠酸的吸附能力。结果显示以MIP3对目标分子的保留能力最强,且当柱温为443K,印迹柱对糠酸相对于糠醛的选择因子可达11.55,显示出较高的选择性能。确定的色谱条件下,MIP3柱能有效分离糠酸-糠醛模拟混合物,糠酸与糠醛的分辨率可达为1.544。吸附等温线结果显示MIP3对糠酸的吸附量远高于对糠醛的吸附量,印迹材料对样品模拟液的吸附情况显示对糠酸具有较强的吸附能力。(3)丹皮酚为模板分子,制备了丹皮酚分子印迹聚合物,利用扫描电镜和红外光谱表征其结构,考察了MIP对目标分子的特异识别性能,探究了其对目标分子及类似物的选择分离能力,测试了其作为气相色谱固定相对气态分子的键合能力,计算得到丹皮酚和相关化合物在固定相上的吸附等温线。结果显示在优化的色谱条件下,印迹柱对丹皮酚的保留因子可达144.2,对丹皮酚的选择因子相对于丁香酚为6.61,呈现出较高的选择保留能力,另外,丹皮酚、丁香酚的混合物能够在分子印迹柱上达到完全分离。丹皮酚及丁香酚在分子印迹聚合物的吸附等温线表明:目标分子与印迹位点具有较强的结合作用,且在相同条件下,丹皮酚的吸附量远高于丁香酚。这些结果都表明:印迹材料对丹皮酚呈现良好吸附选择性能。(4)桃金娘烯醛为模板分子,纳米TiO2为载体,采取表面印迹技术制备出桃金娘烯醛表面印迹材料,采取SEM及红外光谱等方法表征结构,结果说明经过TiO2表面修饰后的分子印迹聚合物已经合成。将制备好的印迹聚合物作为气相色谱固定相,测试其对气态分析质的各种性能。测试了印迹材料对目标分子的保留能力及选择性,在确定的色谱条件下,印迹柱对桃金娘烯醛的保留因子可达63.4,远远大于对松油醇的保留因子;探究了其表面印迹位点与目标分子的键合能力,由目标分子在不同进样体积下的气相色谱图,计算并绘制出桃金娘烯醛及相似物在固定相上的吸附等温线,表明桃金娘烯醛印迹聚合物表面印迹位点与目标分子的键合作用要强于松油醇,且对桃金娘烯醛的吸附量也高于松油醇。
[Abstract]:In this paper, the molecular imprinting polymer was prepared by using toluene, furfuryl acid, paeonol and myrcaldehyde as the target molecule, and the structure of the molecularly imprinted polymer was tested by different methods, and the structure was used as the stationary phase of gas chromatography. The retention and adsorption of gaseous template molecules were studied by reverse-phase gas chromatography. The selective effect and bonding ability of fixed relative gaseous target molecules were investigated, the adsorption isotherms of the target molecules on the blots were measured, and the actual adsorption of the molecularly imprinted polymer to the template in the sample was tested. The specific abstract is as follows: And (1) using toluene as a pore-forming agent (as a template molecule) in combination with a photopolymerization method, and preparing a toluene-imprinted polymer uniform microsphere by using a tetravinyl benzene-based monomer as a functional monomer. The structural characteristics of the microspheres were determined by a nitrogen adsorption method and an optical microscope. The selective retention of the gaseous toluene molecules and related compounds was studied by reversed-phase gas chromatography, and the isothermal bonding ability of the imprinted material and the control polymer to the template was discussed. The results show that the toluene-imprinted (MIP3) gas chromatographic column has a high selectivity to the gaseous toluene molecule, and the retention factor and the imprint factor of toluene are as high as 68.42 and 7.049, respectively, under the optimized chromatographic conditions. The selection factors for toluene were 4.821 and 5.370, respectively, and the simulated mixture of toluene, benzene and p-xylene was effectively separated (the resolution of toluene to para-xylene and benzene was 5.138 and 1.762, respectively). The adsorption isotherms of the toluene-imprinted microspheres on the gaseous toluene showed a type 鈪，
本文编号：2450302
[Abstract]:In this paper, the molecular imprinting polymer was prepared by using toluene, furfuryl acid, paeonol and myrcaldehyde as the target molecule, and the structure of the molecularly imprinted polymer was tested by different methods, and the structure was used as the stationary phase of gas chromatography. The retention and adsorption of gaseous template molecules were studied by reverse-phase gas chromatography. The selective effect and bonding ability of fixed relative gaseous target molecules were investigated, the adsorption isotherms of the target molecules on the blots were measured, and the actual adsorption of the molecularly imprinted polymer to the template in the sample was tested. The specific abstract is as follows: And (1) using toluene as a pore-forming agent (as a template molecule) in combination with a photopolymerization method, and preparing a toluene-imprinted polymer uniform microsphere by using a tetravinyl benzene-based monomer as a functional monomer. The structural characteristics of the microspheres were determined by a nitrogen adsorption method and an optical microscope. The selective retention of the gaseous toluene molecules and related compounds was studied by reversed-phase gas chromatography, and the isothermal bonding ability of the imprinted material and the control polymer to the template was discussed. The results show that the toluene-imprinted (MIP3) gas chromatographic column has a high selectivity to the gaseous toluene molecule, and the retention factor and the imprint factor of toluene are as high as 68.42 and 7.049, respectively, under the optimized chromatographic conditions. The selection factors for toluene were 4.821 and 5.370, respectively, and the simulated mixture of toluene, benzene and p-xylene was effectively separated (the resolution of toluene to para-xylene and benzene was 5.138 and 1.762, respectively). The adsorption isotherms of the toluene-imprinted microspheres on the gaseous toluene showed a type 鈪，
本文编号：2450302
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