【作者】 黄成；

【导师】 周光明；

【作者基本信息】 西南师范大学 ， 分析化学， 2005， 硕士

【摘要】 目前,高效液相色谱(HPLC)法由于在各种干扰物质中对分析物具有极高的分离效率已成为最有效的分离方法之一。将具有高灵敏度的化学发光分析法与具有高分离效率的高效液相色谱(HPLC)分离法相结合已引起了国内外分析化学家的极大兴趣,成为从上个世纪80年代末至今分析化学研究的一大热点。毫无疑问,高效液相色谱分离技术与化学发光检测法的联用将在环境科学、生命科学、药物科学及临床医学上得到愈来愈广泛的应用。 本文包括两个部分。第一部分是综述,这部分结合化学发光分析法,评述了近十年高效液相色谱及其与化学发光柱后检测技术在药物分析和环境分析中的应用。 第二部分是研究报告。第一节是高效液相色谱及其与化学发光柱后检测技术在环境分析中的应用,研究了苯酚和U,N-二甲基苯胺-铁氰化钾-鲁米诺的高效液相色谱-化学发光体系的发光行为,建立了简单、灵敏、快捷测定N,N-二甲基苯胺、同时测定苯酚的HPLC-CL新方法,并应用于环境分析中;同时,应用高效液相色谱最常用的紫外检测器,研究了苯胺的分离分析方法,成功应用于染料靛蓝中残留苯胺的快速分析测定。第二节是高效液相色谱及其与化学发光柱后检测技术在药物分析中的应用,研究了四环素、土霉素的HPLC-CL方法,应用于动物肝组织中四环素、土霉素残留量的测定;并研究了用离子抑制-反相高效液相色谱法快速测定落羽杉中的莽草酸的新方法。 1.高效液相色谱-柱后化学发光同时测定废水中的N,N-二甲基苯胺和苯酚更多还原

【Abstract】 At present, high performance liquid chromatography (HPLC) has mostly been used to enhance the selectivity of analytical methods, because of its high efficiency for separation of analytes from various interfering substances. One of the major research areas about HPLC involves the development of sensitive detection methods. Significantly more sensitive detection can be realized by HPLC when the analytes are subjected to the use of chemiluminescence (CL) detection. The chemiluminescence (CL) detection system combined with HPLC separation method can offer excellent analytical selectivity and sensitivity. No doubtably, chemiluminescence linked to HPLC will be widely applied in environmental science, biological science, pharmaceutical science and clinical science.The thesis consists of two parts. One is a review related to the application of HPLC with post-column chemiluminescence detection to environmental and pharmaceutical samples. Emphasis is taken on the development in the recent ten years.The other is research reports which is composed of 4 components as follows. 1) simultaneous determination of N, N-Dimethylaniline and phenol in wastewater by high-performance liquid chromatography with chemiluminescence detection; 2) rapid determination of rudimental trace aniline in indigotine by reverse phase HPLC; 3) determination of the levels of tetracycline and oxytetracycline residues in liver tissue by HPLC-CL; 4) rapid determination of Shikimic acid in taxodium distichum by ion-suppression reversed-phase HPLC. 1. Simultaneous Determination of N, N-Dimethylaniline and Phenol inWastewater by High-Performance Liquid Chromatography with Chemilumineseence DetectionA method using HPLC-CL linkage was developed for simultaneous determination of N, Af-dimethylaniline and phenol in wastewater, based on the strong sensitive chemilumineseence of the luminol-K3Fe (CN) 6 systems in alkaline medium. The separation was carried out on a Hypersil ODS column with a mobDe phase of ethanol-0.01% triethylamine (2:1,V/V). The linear ranges for N, W-dimethylaniline determinations were 2.0 X 10~7 g/mL~2.5 X10"5 g/mL and 4.0 X10’5 g/mL~ 1.5 X10"4 g/mL with a detection limit (3a) of 1.20 X10"* g/mL. The relative standard deviation for 5.0 X lO^g/mL A^W-dimethylaniline was 1.4% (n = 6).The range for phenol was from 5.1X10’7g/mLtol.3X10^ g/mL, and a detection limit (3a) of^SXlO^g/mL could be obtained. The method can be useful for the determination of N, AT-dimethylaniline and phenol in some environmental samples.2. Rapid Determination of Rudimental Trace Aniline in Indigotine by Reverse Phase HPLCAn accurate and reliable reverse phase HPLC method was established for the determination of rudimental trace aniline in indigotine. Aniline can be separated on YWG-C18 (5um,300mmx5mm ID) column by using methanol: water=70:30 as mobile phase with UV detector at a wavelength of 285nm.The standard curve was linear in the concentration range 6.92 X 10"8gAnL~ 3.59 X lO^g/mL and the correlation coefficient was 0.999 7. The recovery and RSD was 98.34%~98.36% and 1.84%~3.03%(n = 5)respectively. The detection limit was 2.02X lO*g/mUS/N= 3). The method has been successfully applied to the determination of rudimental trace aniline in indigotine, which proved to be simple and rapid.3. Determination of the Levels of Tetracycline and Oxytetracycline Residues in Liver Tissue by HPLC-CLAn HPLC-CL linkage method was developed for simultaneous determination of Oxytetracycline and tetracycline in animal liver tissues, based on the strong sensitive chemilumineseence of the CH3CN-H2O2 system in alkaline medium. The separation was carried out on a Hypersil ODS column with a mobile phase of CH3CN: HCON更多还原