【作者】 张远馥；

【导师】 王金中；

【作者基本信息】 河南大学 ， 分析化学， 2008， 硕士

【摘要】 发光分析是分子发光光谱分析的简称,主要包括化学发光分析(生物发光分析),分子荧光和磷光三大部分。荧光是一种光致发光现象,它是最灵敏的分析技术之一,并且具有选择性高、取样量少、简便快速的特点。本文综述了近年来荧光分析法在药物分析中的应用与研究。本研究工作中,主要利用荧光衍生法及配合法对抗生素类药物进行测定。各项研究工作简述如下:一荧光衍生法在药物检测中的应用1、注射用的头孢曲松钠含量的测定头孢曲松钠溶液本身不发荧光,它与Fe3+在一定条件下发生反应生成荧光物质。以此建立新的测定头孢曲松钠含量的荧光分析方法。其反应生成的荧光物质的最佳激发波长为378 nm、发射波长为487 nm。用该法测定头孢曲松钠,线性范围为1～10 mg·L-1,检出限0.23 mg·L-1,回收率为100.4%。结果令人满意。2、注射用的头孢他啶含量的测定头孢他啶与Fe3+在一定条件下发生配合反应生成强荧光物质,以此建立新的测定头孢他啶含量的荧光分析方法。其反应生成的荧光物质的最佳激发波长为370 nm、发射波长为432 nm。用该法测定头孢他啶,线性范围为2.5～25.0 mg·L-1,检出限0.38 mg·L-1,回收率为101.3%。二荧光配合法在药物检测中的应用研究1、荧光法测定头孢拉定胶囊含量头孢拉定在酸性环境中发出弱的荧光,但是它与Au(Ⅲ)在一定条件下发生配合反应生成荧光物质,发出强的荧光。以此建立新的测定头孢拉定含量的荧光分析方法。其反应生成的荧光物质的最佳激发波长为353 nm、发射波长为433 nm。用该法测定头孢拉定,其线性范围为1～25.0 mg·L-1,检出限0.30 mg·L-1,回收率为101.7%。2、荧光法测定针剂头孢噻肟钠的含量头孢噻肟钠与Fe3+在一定条件下发生反应生成荧光物质,以此建立新的测定头孢曲松钠含量的荧光分析方法。其反应生成的荧光物质的最佳激发波长为370 nm、发射波长为480 nm。用该法测定头孢曲松钠,线性范围为1.0～24.0 mg·L-1,检出限0.18 mg·L-1,回收率为100.4%。本法已用于头孢噻肟钠针剂的测定,结果与药典法基本一致。三阻抑动力学荧光法测定头孢拉定在弱酸性介质中,头孢拉定能够阻抑铈(IV)氧化光泽精的荧光猝灭反应,从而建立了阻抑动力学荧光法测定头孢拉定含量的新方法,头孢拉定的质量浓度与荧光强度的变化在2.5~50 mg·L-1范围内呈良好线性关系,检出限1.09 mg·L-1。该方法简便、快速,并应用于药物制剂中头孢拉定含量的测定,结果令人满意。四共振瑞利散射法测定阿米卡星在酸性介质中,络天青S和硫酸阿米卡星自身的共振瑞利散射峰(RRS)较弱,两者混合后溶液的RRS显著增强,并产生了新的RRS光谱。最大RRS峰位于414 nm处,而且在1.2～10.0 mg·L-1范围内,AMK的浓度与散射强度变化量(ΔIRRS)成正比。检出限为0.19 mg·L-1,平均回收率为100.2%。更多还原

【Abstract】 Luminescence analysis is the abbreviation of molecular spectrum,composing of molecular fluorescence phosphorescence and chemluminescence analysis(including bioluminescence).Fluorescence is a photoluminescence phenomenon. It is one of the most sensitive analysis techniques. There are several characteristics of fluorescence, which are high selective, less sampling, simple and rapid. The paper Reviews the application of fluorescence in pharmaceutical analysis.In this paper, we determine the amount of Cephalosporins by derivative fluorescence spectroscopy with complex reaction. The thesis consists of four parts:Part 1 Determination of Pharmaceutical by Derivative Fluorescence spectroscopyChapter 1 Determination of Ceftriaxone in Injection by Fluorescence s pectroscopyCeftriaxone sodium does not have the feature of fluorescence. The new method is based on a chromogenic reaction of ceftriaxone sodium with ferric under the condition which produces a fluorescence substance. The best emission wavelength and excitation wavelength of the fluorescence substance are 378 nm and 487 nm. The linear range of the determination is 1-10 mg·L-1. The detection limit for ceftrisxone sodium is 0.23 mg·L-1. The average recovery is 100.43%. The people were satisfied with the result.Chapter 2 Fluorimetric determination of ceftazidime in injectionThe new method is based on a chromogenic reaction of ceftazidime sodium with ferric under the condition which produce a strongly fluorescence substance. The best emission wavelength and excitation wavelength of the fluorescence substance are 370 nm and 432 nm. The linear range of the determination is 2.5-25.0 mg·L-1. The detection limit for ceftazidime sodium is 0.38 mg·L-1. The average recovery is 101.4%.Part 2 Fluorimetric study on the Complex Reaction in Pharmaceutical analysisChapter 1 Study on Fluorimeritric Determination of Cefradine capsuleCefradine emit weak fluorescence in acid sodium.The new method is based on a chromogenic reaction of Cefradine sodium with Au (Ⅲ) under the condition which produce a strongly fluorescence substance. The best emission wavelength and excitation wavelength of the fluorescence substance are 353 nm and 433 nm. The linear range of the determination is 1-25.0 mg·L-1. The detection limit for Cefradine sodium is 0.30 mg·L-1. The average recovery is 101.7%.Chapter 2 Study on Fluormeritric Determination of Cefotaxime Injection The new method is based on a chromogenic reaction of cefotaxime sodium with ferric under the condition which produces a fluorescence substance. The best emission wavelength and excitation wavelength of the fluorescence substance are 370 nm and 480nm. The linear range of the determination is 1.0-24.0 mg·L-1. The detection limit for ceftrisxone sodium is 0.18 mg·L-1.The average recovery is 100.43%. The method has been used to determination in tablets and the results were in good agreement with those obtained by classical method.Part 3 Inhibitory Kinetic Fluorimetric Determination of Cefradine An inhibitory kinetic fluorimetric method is reported for the determination of Cefradine. The proposed method is based on the inhibitory effect of Cefradine on the reaction of (NH4)2Ce(NO3)6 oxidation of Lucigenin in Na2SO4-H2SO4 buffer solution medium. The detection limit for Cefradine is 1.09 mg·L-1.The linear range of the determination is 2.5~50 mg·L-1. This method has been used successfully to determine Cefradine capsules.Part 4 Study on the Determination of Amikin with Rayleigh Scattering SpecterumIn weak acid medium, Amikin or ChromeAzcerol S alone can only produce very weak resonance Rayleigh scattering (RRS) signal. However, when AMK and CAS react with each other to form the ion association complexes, the RRS intensity can be enhanced greatly, which gives a new RRS spectrum The maximum scattering peak is at 414 nm and there is a linear relationship between the RRS intensity and the AMK concentration in the range of 1.2～10.0 mg·L-1. The detection limit for amikin is 0.19 mg·L-1.The average recovery is100.2%.更多还原