β—环糊精键合滤纸在固相萃取固体基质室温磷光分析中的应用

【作者】 王培龙；

【导师】 朱若华；

【作者基本信息】 首都师范大学 ， 分析化学， 2005， 硕士

【摘要】 多环芳烃和含氮类杂环物质具有强致癌,致变,致畸的作用。由于它们的稳定性,疏水性和亲油性,使得它们能够广泛的存在环境中,难以降解,且容易沉积的底泥和生物体中,因此它们在水环境中的含量特别低,这就使得对于它们的分析检测有很大的困难。固相萃取固体基质室温磷光分析是针对多环芳烃,多氯联苯的分析检测建立的一种新方法。本文分五章对固相萃取-固体基质室温磷光分析进行了研究: 第一章详细介绍了固相萃取-固体基质室温磷光分析的原理,应用和展望。详细叙述了室温磷光的发光机理,影响因素和固相萃取的原理,装置和填料以及固相萃取固体基质室温磷光分析的应用及发展。 第二章研究建立了β-环糊精修饰滤纸的合成方法。优化了合成条件（包括合成方式,环氧氯丙烷用量,活化时间和滤纸种类等）,考察了修饰滤纸对20种有机物质的室温磷光的增强效果,结果表明β-环糊精修饰滤纸能有选择的增强多种多环芳烃和含氮杂环类物质的室温磷光强度,大大提高它们检测的灵敏度。 第三章研究建立了以β-环糊精修饰滤纸为基质的固相萃取固体基质室温磷光测定多环芳烃中芴和苊的分析方法。详细的考察了芴和苊在修饰滤纸上室温磷光条件。研究了修饰滤纸在固相萃取中的应用,且考察了影响固相萃取的各种因素。在优化条件下,修饰滤纸对芴和苊的富集倍数达到100倍以上。将此方法用于环境水样中的芴和苊的测定,回收率达到90%以上,相对标准偏差（RSD）小于7.3%。 第四章研究建立了固相萃取固体基质室温磷光对含氮类杂环物质中咔唑,7,8—苯并喹琳和菲啶分析检测的方法。考察了咔唑,7,8—苯并喹琳和菲啶在修饰滤纸上室温磷光测定条件,研究了它们在修饰滤纸上的饱和度和萃取效果,并且考察了多环芳烃和其他的氮杂环类物质对它们的干扰。通过固相萃取之后,咔唑,7,8—苯并喹啉和菲啶的检测限能降低两个数量级,分别为9.1×10^-11,8.3×10^-10和7.8×10^-10molL^-1。最后将此方法用于环境水样中的咔唑,7,8—苯并喹啉和菲啶的测定回收率介于86.1%和109.3%之间。 第五章主要从定性和定量两方面研究了主成分分析和模式识别在SS-RTP中更多还原

【Abstract】 Polycyclic aromatic hydrocarbons （PAHs） and nitrogen heterocyclic compounds （NHCs） are of carcinogenesis and deformity and unfavorable to human health. Their chemical and physical stability makes them ubiquitous in the environment, particularly in the aquatic ecosystem, so oceans, rivers, and lakes act as ultimate PAHs and NHCs environment reservoirs. Due to their hydrophobic and lipophilic character, PAHs and NHCs tend to accumulate in sediments and biota and thus their concentrations in water samples are extremely low. The partitioning process into sediment and biota results in low water concentration levels. Therefore, high sensitive analysis techniques combine with the preconcentration process for the determination of PAHs and NHCs in the water samples are often required. The solid phase extraction - room temperature phosphorescence（SPE-RTP） is an effective method for the determination of PAHs, PCBs and so on. So our works focus on the further development and perfection of SPE-RTP.In chapter 1, the mechanism, application and prospect of SPE-RTP were introduced in detail. The luminescence mechanism of RTP, impact factor and the principle of SPE, instrument and the application and development of SPE-RTP was described completely.In chapter 2, the experimental method of p-cyclodextrin（p-CD） modified chromatography filter paper was developed. Experimental conditions of beta-cyclodextrin bonded chromatography filter paper was optimized, includingsynthetical mode, the dosage of epichorohydrin, activation time and the kind of filter paper, and RTP behavior of 16 organics on the bonded filter paper were studied. The result indicated that the intensities of RTP of several PAHs and NHCs were selectively intensified on the modified filter paper, and the sensitivities of determination of them were enhanced.In chapter 3, the determination method of SPE-RTP for fluorene and acenaphthene with beta-cyclodextrin bonded filter paper substrate was developed. The RTP condition of fluorene and acenaphthene on the bonded filter paper was examined in detail. Application of bonded filter paper in SPE and the impact factor of SPE were studied. Under the optimized condition, the enrichment efficiency of fluorene and acenaphthene were more than 100 times. This method was used into determination of fluorene and acenaphthene in environmental water samples, the recovery >90%, the relative standard deviate（RSD） < 7.3%, it indicated that the reliability of the developed method.In chapter 4, the analytical mean of SPE-RTP for carbazole, 7,8-benzoquinoline and phenanthridine with beta-cyclodextrin bonded filter paper was developed. The RTP conditions of carbazole, 7,8-benzoquinoline and phenanthridine and saturated volume and enrichment efficiency on the modified filter paper were examined, and the interferences of PAHs and other NHCs for carbazole, 7,8-benzoquinline and phenanthridind were examined , too. Through a SPE procedure, the limit of detection （LOD） of carbazole, 7,8-be（?）oquinoline and phenanthridine were improved twoorders of magnitude, wh（?） were found to be 9.1×10^-11 , 8.3×10-10and7.8×10-10molL-l respectively. The proposed method was applied for the analysis of water samples. The recoveries of carbazole, 7,8-benzoquinoline and phenanthridine in water samples was from 86.1% to 109.3%.In chapter 5, the application of pattern recognition and principle component analysis in the solid substrate room temperature phosphorescence was studied from both qualitative and quantitative perspective. The performance effective of principle component analysis in the course of dealing with SS-RTP of PAHs and NHCs mixtures was assessed primarily. The results showed that fluorene, acenaphthene, carbazole, 7,8-benzoquinoline and phenanthridine could be identified from arbitrary mixture each other by applying RTF artificial neural net. It indicated that it feasible in the mixtures analysis.更多还原