【作者】 付志锋；

【导师】 章竹君；

【作者基本信息】 西南师范大学 ， 分析化学， 2004， 硕士

【摘要】 本论文主要介绍了N-溴代琥珀酰亚胺和高锰酸钾化学发光体系在药物分析中的应用，全文由两章组成。 第一章是N-溴代琥珀酰亚胺（NBS）化学发光体系的应用，全章分为五节。 第一节综述了N-溴代琥珀酰亚胺化学发光体系的研究进展，对该体系的分析应用及机理研究的状况进行了详细介绍。 第二节研究了2-氨基丁酸的流动注射化学发光分析法。研究发现2-氨基丁酸在碱性条件下被NBS氧化，产生微弱的化学发光，而荧光素的存在可以大大增强发光强度。利用这种现象，结合流动注射技术，建立了检测2-氨基丁酸的新方法。2-氨基丁酸浓度在3.0×10⁷～1.0×10^-4g／mL范围内与化学发光强度呈良好的线性关系；对5.0×10^-6g／mL的2-氨基丁酸进行11次平行测定，相对标准偏差（RSD）为2.0％；根据IUPAC建议，计算出2-氮基丁酸检测限（3σ）为8.0×10^-8g／mL。将本法用于化学去龋剂中2-氨基丁酸含量的测定，结果满意。 第三节研究了沙丁胺醇的流动注射抑制化学发光分析法。研究发现沙丁胺醇对NBS-荧光素化学发光体系有着强烈的抑制作用，据此可以建立检测该药物的流动注射抑制化学发光分析法。方法的线性范围为8.0×10^-8～1.0×10^-5g／mL；检测限（3σ）为2.6×10^-8g／mL；对3.0×10^-7g／mL的沙丁胺醇进行了11次平行测定，相对标准偏差为3.0％。 第四节研究了流动注射化学发光系统在庆大霉素的溶出度研究中的应用。本文利用NBS-荧光素-庆大霉素体系的化学发光行为，结合流动注射技术，建立了一种在线监测药物庆大霉素片的溶出过程的新方法。该法灵敏，简单，快速，自动化程度高。 第五节研究了NBS-鲁米诺体系抑制化学发光分析法在检测氨茶碱和氨甲苯酸中的应用。NBS和鲁米诺反应产生强烈的化学发光，而氨茶碱和氨甲苯酸可以显著抑制发光。基于此，结合流动注射技术，建立了检测这两种药物的新方法。该法检测氨甲苯酸和氨茶碱的线性范围分别为2.0×10^-8～1.0×10^-6g／mL和1.0×10^-7～7.0×10^-6g／mL；对2.0×10^-7g／mL的氨甲苯酸和1.0×10^-6g／mL的氨茶碱平行测定11次，相对标准偏差分别为 内容摘要2.6%和3。%;根据Iu队c建议，计算出氨甲苯酸和氨茶碱的检测限分别为7.0 x10’9g/mL和3.4xl0一sg/mL。本法己成功用于药物制剂中的氨甲苯酸和氨茶碱的测定。 第二章是高锰酸钾化学发光体系的分析应用，全章分为三节。 第一节综述了1994年以来高锰酸钾化学发光体系的研究进展，比较全面地介绍了近十年来该体系的发展现状。 第二节研究了高锰酸钾一甲醛体系测定[l9}垛美辛的化学发光分析法。研究发现，在多聚磷酸介质中，高锰酸钾氧化叫垛美辛产生化学发光，甲醛的存在可显著增大发光强度。幕于此，建立了一种灵敏检测叫垛美辛的流动注射化学发光分析方法。本方法线性范l^「I为2.ox 10一9一2 .ox 10一6 92，。L;对2 .oxlo一‘92:nxjt/J，l引l垛美辛进行一l次平行测定，相对标准偏差为2.3%;根据Iu队c建议，算出检测限为8.0xl0一’0 g/lnL（3a）。本法己成功用于测定胶囊中的叫垛美辛含量。 第三节研究了高锰酸钾一甲醛一肾上腺色踪体系的化学发光行为，对影响发光强度的诸因素进行了实验探讨，并以此建立了一种非常灵敏的检测肾上腺色踪的流动注射化学发光分析法。方法的线性范围为7.0xl0一‘。一1.oxlo“，g/mL;对1.0X10一8以mL的样品连续进行11次平行测定，相对标准偏差为2.5%;根据IU队C建议，算出本法检测限为2 .ox 10一1092一nL（3a）。更多还原

【Abstract】 Application of N-bromosuccinimide and permanganate chemiluminescence system in pharmaceutical analysis is described in this paper. Two chapters arc contained in this paper.Chapter 1 describes the application of N-bromosuccinimide (NBS) chemiluminescence system, and five sections are contained in this chapter.The first section reviews the development of N-bromosuccinimide CL system. Application and mechanism research of this system arc described in detail in this section.The second section recommends a flow injection CL analysis method for the determination of 2-aminobutyric acid. The method is based on the CL emitted during the oxidation of 2-aminobutyric acid by N-bromosuccinimide in alkaline medium in the presence of fluorescent compound as energy-transfer. The detection limit is 8.0 X10-8 g/mL(3 o ), the linear range of determination is 3.0 X 10-7 - 1.0 X 10-4 g/mL with the relative standard deviation of 2.0 %(C=5 X 10-6g/mL, n=11). The recommended method has been successfully used for analysis of caries removel system with a satisfactory result.The third section describes a CL method for the determination of salbutamol. It is based on the strong inhibition of salbutamol on the CL of the reaction of NBS and fluorescein in alkaline medium. Various factors affecting the CL emission are studied in detail. The possible mechanism is also discussed. The decrease of CL emission is linear with salbutamol in the range of 8.0X 10-8~1.0X 10-5g/mL. The detection limit is 2.6X 10-8g/mL and the RSD is 3.0 %(C=3.0X 10-7g/mL, n=11). It has been successfully used for the determination of salbutamol in pharmaceutical preparation.The fourth section describes a flow-injection system for automated dissolution testing of gentamycin tablets with CL detection. A simple and sensitive flow-injection CL system forautomated dissolution testing is described and evaluated for monitoring of dissolution profiles of gentamycin tablets. The dissolution profiles of gcntamycin fast-release tablets was determined, which demonstrates the stability, great sensitivity, large dynamic measuring range and robustness of the system.The fifth section presents a novel and sensitive CL method for the determination of aminomethylbenzoic acid and aminophylline coupled with flow-injection analysis technique. It is based on the inhibition effect of the studied drugs on the CL emission of NBS-luminol system. Under the optimum conditions, the decreased CL intensity is linear with the concentration of aminomethylbenzoic acid in the range of 2.0x10-8 to 1.0xl0-6gml-1 and with the concentration of aminophylline in the range of 1.0x10-7 to 7.0xl0-6gml-1. respectively. The detection limit is 7.0xl0-9gml-1 for aminomethylbenzoic acid (3o) and 3.4x10-8gml-1 for aminophylline (3o). The relative standard deviations for 11 parallel measurements of 2.0x10-7gml-1 aminomethylbenzoic acid and 1.0x10-6gml-1 aminophylline are 2.6 and 3.0 %, respectively. The proposed methods have been applied for the determination of the studied drugs in their pharmaceutical formulations with satisfactory results.Chapter 2 describes the application of permanganate chemiluminescence system, and three sections are contained in this chapter.The first section reviewed the development of acidic permanganate CL system since 1994.The second section recommends a sensitive flow injection CL method for the determination of indomethacin. It is based on CL emitted during the oxidation of indomethacin by KMnO4 in polyphosphoric acid medium. CL can be greatly enhanced in the presence of formaldehyde. The method permits the determination of indomethacin over a concentration range of 2.0x10-9~1.0x10-6 g/mL with a RSD of 2.3 % for the determination of 1.0x10-8 g/mL indomethacin (n = 11). The recommended method is suitable for automatic and continues analysis. The recommended method has been successfully used for analysis of commercial formulations without any sample pre-treatment.The third section proposes a flow injection analysis method for the determination of carbazochrom更多还原