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1、河南大学 硕士学位论文 发光分析在头孢类抗生素药物检测中的应用研究 姓名：王珏 申请学位级别：硕士 专业：分析化学 指导教师：屈建莹 2011-05 摘 要 I 摘 要 本论文分为两部分：综述和研究报告。第一部分综述了荧光分析法和化学发光分析 法在药物分析中的应用。第二部分：在研究报告中利用阻抑动力学荧光法和流动注射化 学发光分析法对几种头孢类抗生素药物进行测定。 1. 流动注射化学发光法测定头孢噻肟钠 基于碱性介质中头孢噻肟钠对鲁米诺-铁氰化钾化学发光体系的增强作用，建立了 流动注射化学发光测定头孢噻肟钠的新方法。 化学发光强度的变化与头孢噻肟钠的质量 浓度在2.410-63.010-4 g
2、/mL范围内呈良好的线性关系，检出限为6.310-7 g/mL，对 3.010-4 g/mL的头孢噻肟钠进行9次平行测定，相对标准偏差（RSD）为1.0。将其用 于头孢噻肟钠针剂的测定，结果令人满意。 2. 纳米金催化化学发光法测定头孢哌酮钠 以硝酸银-鲁米诺为基本体系，金纳米粒子为催化剂，建立了新的测定头孢哌酮钠 的分析方法，在优化的实验条件下，用该法测得头孢哌酮钠的线性范围为 5.010-79.010-4 g/mL， 检出限为1.010-7 g/mL， 相对标准偏差为1.6 （c=3.010-6 g/mL， n=11）。将其用于药物制剂中头孢哌酮钠含量的测定，结果令人满意。 3. 流动注射
3、化学发光法测定头孢他啶 在碱性条件下，头孢他啶对金纳米粒子催化高锰酸钾-鲁米诺化学发光体系的发光 强度具有明显的增敏作用，基于此建立了一种化学发光法测定头孢他啶的新方法。在最 佳实验条件下，用该法测定头孢他啶的线性范围为 3.010-85.010-5 g/mL，检出限为 1.010-8 g/mL，相对标准偏差为 2.0（c=4.010-6 g/mL，n=11） ，将其用于药物制剂中 头孢他啶含量的测定，测得平均回收率为 99.2%，结果令人满意。该法简便、快速、灵 敏，且线性范围宽。 4. 阻抑动力学荧光法测定针剂中头孢哌酮钠的含量 在弱酸性介质中， 头孢哌酮钠能够阻抑过硫酸钾减弱曙红 Y 褪
4、色， 由此建立了阻抑 动力学荧光法测定头孢哌酮钠含量的新方法。 头孢哌酮钠的质量浓度与荧光强度的变化 在 1.010-62.010-5 g/mL 范围内呈良好线性关系（r=0.9986） ，方法的检出限为 3.810-8 g/mL，其相对标准偏差（RSD）为 2.0。该法简便、快速、可靠，可用于药物制剂中 发光分析在头孢类抗生素药物检测中的应用研究 II 头孢哌酮钠含量的测定，结果令人满意。 5. 阻抑动力学荧光法测定胶囊中头孢拉定的含量 在碱性介质中，头孢拉定能够阻抑过硫酸钾减弱达旦黄的荧光，基于此建立了阻抑 动力学荧光法测定头孢拉定含量的新方法。在优化条件下，用该法测定头孢拉定的线性 范围
5、为 5.010-71.010-5 g/mL， 检出限为 5.610-8 g/mL， 对浓度为 5.010-6 g/mL 的头孢 拉定进行 11 次平行测定，相对标准偏差（RSD）为 1.1%。将其用于药物制剂中头孢拉 定含量的测定，结果令人满意。 关键词：阻抑动力学荧光法，流动注射，化学发光，头孢哌酮钠，头孢拉定，头孢噻肟 钠，头孢他啶，曙红 Y，达旦黄，鲁米诺，过硫酸钾，纳米金 ABSTRACT III ABSTRACT This thesis consists of two parts: review and research report. The review involves the
6、 application of fluorimetry and chemiluminescence in pharmaceutical. The research report is focused on the study of the determination of inhibitory kinetic fluorimetric analysis and FIA-chemiluminescence analysis in antibiotics. 1. FIA-Chemiluminescence Determination of Cefotaxime Sodium A new metho
7、d for determination of cefotaxime sodium was developed using flow injection chemiluminescence analysis based on that cefotaxime sodium could greatly enhance the emission intensity of the chemiluminescence reaction of K3Fe(CN)6 and luminol in alkaline medium. The relative chemiluminescence intensity
8、is proportional to cefotaxime sodium concentration over the range 2.410-63.010-4 g/mL with a detection limit of 6.310-7 g/mL. 9 times of parallel determination of 3.010-4 g/mL cefotaxime sodium show that the relative standard deviation (RSD) is 1.0%. It has been satisfactorily applied to determine c
9、efotaxime sodium in injection. 2. Determination of Cefoperazone Sodium with Chemiluminescence catalyzed by Nanogold Particles In alkaline medium, the system of nanogold catalyzed silver nitrate-luminol has a very strong chemiluminescence. Cefoperazone sodium can inhibit emission of this system. A ne
10、w analytical method for determination of cefoperazone sodium was established based on this. In the optimum conditions, the linear range was 5.010-79.010-4 g/mL with the detection limit of 1.010-7 g/mL. The relative standard deviation (RSD) was 1.6% for 3.010-6 g/mL cefoperazone sodium (n=11). This m
11、ethod is simple, rapid with broad linear range. It has been satisfactorily applied to determine cefoperazone sodium in injection. 3. Determination of Ceftazidime by Flow Injection Chemiluminescence In alkaline medium, gold nano-particles could catalyze the chemiluminescence (CL) of the luminol-potas
12、sium permanganate system, and ceftazidime could enhance CL intensity of this system. Based on this, a flow injection CL method for determination of ceftazidime was established. In optimized condition, the linear range of determination was 3.010-85.010-5 g/mL with the detection limit of 发光分析在头孢类抗生素药物
13、检测中的应用研究 IV 1.010-8 g/mL. The relative standard deviation (RSD) was 2.0% for 4.010-6 g/mL ceftazidime (n=11). It has been satisfactorily applied to determine ceftazidime in injection. This method is simple and rapid with broad linear range. 4. Inhibitory Kinetic Fluorimetric Determination of Cefoper
14、azone Sodium in Injection Based on the inhibitory effect of cefoperazone sodium on the oxidation reaction of K2S2O8 for eosin-Y in weak acid medium, an inhibitory-kinetic fluorimetric method is developed for the determination of cefoperazone sodium. The linear range of the determination is 1.010-62.
15、010-5 g/mL (r=0.9986) with the detection limit of 3.810-8 g/mL. And the relative standard deviation (RSD) is 2.0. This method is simple, rapid and credible, which can be used for the determination of cefoperazone sodium in pharmaceutical formulation. 5. Inhibitory Kinetic Fluorinetric Determination
16、of Cephradine in Capsule Based on the inhibitory effect of cephradine on the reaction of K2S2O8 for titan yellow in alkaline medium, an inhibitory-kinetic fluorimetric method is developed for the determination of cephradine. In the optimum conditions, the linear range was 5.010-71.010-5 g/mL with the detection limit of 5.610-8 g/mL. The relative standard deviation (RSD) was 1.1% for 5.010-6 g/mL cephradine (n=11). This method is simple, rapid
