【作者】 张子瑜；

【导师】 陈慧；

【作者基本信息】 西北师范大学 ， 分析化学， 2003， 硕士

【摘要】 流动注射化学发光法作为一种有效的痕量分析技术，因具有灵敏度高，线性范围宽，而且分析快速、重现性好、自动化程度高等特点，在分析化学领域得到了迅速发展。本文系统评述了该法在药物分析方面的应用，并着重报道了利用罗丹明B—Ce（Ⅳ）—H₂SO₄这一新的化学发光体系建立的尿酸、芦丁及叶酸的流动注射化学发光检测法。论文分为四个部分： 第一部分 流动注射化学发光法在药物分析中应用研究的进展 简要介绍了流动注射化学发光分析法的建立、基本原理及其发展概况。系统评述了自1985年以来流动注射化学发光法在药物分析中取得的研究进展。 第二部分 罗丹明B-Ce（Ⅳ）-H₂SO₄化学发光体系检测尿酸 尿酸对罗丹明B-Ce（Ⅳ）-H₂SO₄体系的化学发光有增敏作用，阳离子表面活性剂CTMAB的存在可进一步增强体系的发光强度，据此建立了利用罗丹明B-Ce（Ⅳ）-H₂SO₄体系测定尿酸的流动注射化学发光新方法。在选定的最佳实验条件下，体系的化学发光与尿酸浓度在1.0×10^-13～5.0×10^-11mol／L之间呈良好的线性关系，检出限为3.7×10^-14mol／L（3σ）。对1.0×10^-11mol／L尿酸标准溶液进行11次平行测定，相对标准偏差为0.74％。本法灵敏度高、选择性好，用于测定尿液中尿酸的含量取得满意结果。 第三部分 罗丹明B-Ce（Ⅳ）-H₂SO₄化学发光体系检测叶酸 利用叶酸对罗丹明B-Ce（Ⅳ）-H₂SO₄化学发光体系的增敏作用建立了测定叶酸的流动注射化学发光新方法。在选定的最佳实验条件下，体系的化学发光与叶酸浓度在3.0×10^-6～3.0×10^-5mol／L之间呈良好的线性关系，检出限为3.0×10^-6mol／L（3σ）。对1.0×10^-5mol／L叶酸标准溶液进行11次平行测定，相对标准偏差为2.3％。本法测定叶酸片剂中叶酸的含量，取得满意结果。 第四部分 罗丹明B-Ce（Ⅳ）-H₂SO₄化学发光体系检测芦丁 芦丁对罗丹明B-Ce（Ⅳ）-H₂SO₄体系的化学发光有显著的猝灭作用，据此建立了利用罗丹明B-Ce（Ⅳ）-H₂SO₄体系测定芦丁的流动注射化学发光新方法。在选定的最佳实验条件下，体系的化学发光与芦丁浓度在3.0×10^-6～1.0×10^-4mol／L之间呈良好的线性关系，检出限为 l．0 XIO知of几u o人对 1．0 XIO”mol几芦了标准溶液进行 11次平行测定，相对标准偏差为1．l％。用本法测定芦丁片剂中芦丁的含量，结果满意。更多还原

【Abstract】 Flow injection (FI) chemiluminescence (CL) analysis has made great progresses in analytical chemistry for its high sensitivity with a wide linear dynamic range, simple instruments, rapidity and reproducibility in signal detection, and being appropriate for on-line analyses. This thesis focuses on the applications of FI-CL method in determination of drugs. The work develops a new FI-CL system for determination of uric acid, folic acid and rutin based on the chemiluminescence reaction of Rhodamine B-Ce (IV) in sulfuric acid media. The main content consists of four parts:Part I FI-CL analysis and analytical applications in determination of drugsThis literature review provides a simple introduction for the development of FI-CL analysis. The mechanism of CL reaction and the basic theory of FIA were discussed briefly. The research progresses of FI-CL method in determination of drugs since 1985 were discussed systematically.Part II Flow-injection chemiluminescence determination of uric acid in human urine by use of the Rhodamine B-Ce(IV) systemA highly sensitive flow injection (FI) chemiluminescence (CL) method has been developed for determination of uric acid based on its enhancement effect of the CL resulting from the reaction of Rhodamine B with Ce (IV) in sulfuric acid media, cationic surfactant CTMAB is used as a sensitizer. The sensitized-type of CL emission is linear over the the logarithm of uric acid concentration in the range of 1.0 #10-13 ~5.0# 10-11 mol l-1, with a detection limit (3σ ) of 3.7×10-14mol l-1. The experimental conditions for the reaction are optimized. The method is applied to the determination of uric acid in human urine with good accuracy and precision.Part III Flow-injection chemiluminescence determination of folic acid by use of the Rhodamine B-Ce(IV) systemA new FI-CL method for the determination of folic acid is described. The method isbased on the enhancement of chemiluminescence of Rhodamine B-Ce(IV)-H2SO4 system by folic acid. The optimum conditions for the CL emission were investigated. With peak height as a quantitative parameter, folic acid can be determined over the concentration range 3.0× l0-6~3.0×10-5 mol l-1 (r=0.9994, n=7) with a detection limit (3a) of 3.0 × 10-6mol l-1 original concentration. The method is successfully applied to the determination of folic acid in a pharmaceutical tablet preparation.Part IV Flow-injection chemiluminescence determination of rutin by use of the Rhodamine B-Ce(IV)- systemA novel FI-CL method has been developed for the determination of rutin based on the CL reaction of Rhodamine B with Ce(IV) in sulfuric acid media. The CL signal produced by the reaction is decreased in the presence of rutin. Under the optimal conditions, the CL intensity is linear to the logarithm of rutin concentration in the range of 3.0×10-6~1.0×10-4 mol l-1, with a detection limit (3σ) of 1 × 10-6 mol l-1. The method is applied to the determination of rutin in pharmaceucal preparations with satisfactory result. The possible reaction mechanism in the system is discussed briefly.更多还原