光度法在胺基类药物分析中的研究与应用

【作者】 许丽晓；

【导师】 王怀友；

【作者基本信息】 山东师范大学 ， 分析化学， 2004， 硕士

【摘要】 药物分析学是整个药学科学领域中一个重要的组成部分。药品质量直接影响人们的身体健康和生命安全，因此，对药品质量进行全面控制，以确保人们用药的安全具有十分重要的意义。光谱、色谱以及光谱-色谱联用技术在药物分析学科领域中是基本的研究手段和方法。近年来，在有机分析和生命科学研究中，光度法应用日趋广泛，紫外可见分光光度法目前仍是药物分析中采用最多的方法之一。优化反应条件，简化操作步骤，提高方法的选择性和降低测定的检出限，仍是光度分析需要解决的问题之一。 本文主要以提高灵敏度和选择性为目的，在建立简捷的药物分析方法方面开展了一系列的研究工作。 利用分光光度法研究了抗生素类药物氨苄西林钠，抗麻风病药物氨苯砜，局部麻醉药盐酸普鲁卡因与1，2—萘醌—4—磺酸钠的显色反应，建立了灵敏简便的分光光度法。该反应将药物的最大吸收波长由紫外区红移至可见区，避免了紫外区杂质的严重干扰。在此反应的基础上，实验了pH值、表面活性剂、有机溶剂、加热时间、放置时间及干扰离子对测定的影响，所建立的方法具有线性范围宽，稳定性好等特点，可成功地用于相关药品含量的测定，与药典方法对照，结果吻合。 多巴胺和硝酸汞的氧化产物与乙二胺发生缩合，其缩合产物是强荧光物质，该产物荧光强度与多巴胺的浓度在0.02～0.60μg／ml范围内成线性关系，据此建立了测定多巴胺的荧光光度分析法。该产物最大激发波长为393nm，最大发射波长为447nm，实验了pH、氧化剂及干扰离子对多巴胺测定的影响。相对标准偏差为4.38％，检出限为18ng／ml，回收率为95.0～106.6％。该法不受肾上腺素和去甲肾上腺素的干扰，选择性好，检出限低，成功用于多巴胺注射液和尿样中多巴胺含量的测定，结果令人满意。 利用荧光光度法研究了卡维地洛的酸碱性质，建立了灵敏、简便的荧光分析法。卡维地洛的激发和发射波长分别为254nm和356nm，实验了有机溶剂、pH、干扰离子及放置时间等因素对卡维地洛测定的影响，相对标准偏差为2.31％，线性范围为0.50～270ng／ml，方法检出限为0.19ng／ml，样品回收率为98.70～102.1％。本法可用于药片中卡维地洛含量的测定。更多还原

【Abstract】 The analysis of druggery is one of the most important components in the pharmacology. The quantity of the druggery affects people’s health and safety directly. Therefore the whole control of druggery plays an important role in the clinic and medical treatment. Spectrophotometry, chromatography and spectrophotometry-chromatography, as the most essential methods in the druggery measurements, have been widely used in the determination of pharmic products. In recent years, Spectrophotometry is developing in the study of organic analysis and life sciences. Obviously, UV-visible Spectrophotometry is one of the methods in the qualitative determination of drugs in the modern instrumental analysis. It is still the questions to be solved in the analysis of druggery to optimize the analytical conditions, improve the selectivity, reduce the detection limit and simplify the procedue.To improve the sensitivity and selectivity, some novel and simple methods for the assay of drugs have been established in my master paper.Spectrophotometric determination of procaine hydrochloride, ampicillin sodium and dapsone is disscussed. Procaine hydrochloride, ampicillin sodium and dapsone can react with 1,2-naphthoquinone-4-sulfonic acid to form salmon pink compound, respectively. Their maximum absorption wavelengtb.es were shifted from the range of ultraviolet to the visible light. Therefore procaine hydrochloride, ampicillin sodium and dapsone can be determined in the range of visible light. In this way, much potential interference may be avoided in the determination of these drugs in biological materials and hemanalysis. These methods are rapid, simple and wider linear range, and can be used for determining procaine hydrochloride, dapsone and ampicillin sodium in injectin solutions of these drugs. The results obtained by these methods agreed with those by the official methods.A sensitive and selective method for the determination of dopamine was studied.Dopamine was oxidized by mercury (II) nitrate and the oxidation product was condensed with ethylene diamine to form a quinoxaline derivative which was strongly fluorescent. The measurement was carried out at 447 nm with excitation at 393 nm. Effects of pH, oxidants, and foreign ions on the determination of dopamine were examined. A linear relationship was obtained between the relative fluorescence intensity and the concentration of dopamine in the range of 0.02 to 0.60 ug/ml, the relative standard deviation is 4.38%. The detection limit is 18 ng/ml, and the recovery is from 95.0 to 106.6%. Dopamine was separated from adrenaline and noradrenaline in urine by thin layer chromatography. This method has low detection limit and can be used for the determination of dopamine in injection and urine samples.The property of carvedilol in acid-alkaline medium was studied by spectrofluorimetry. A simple, rapid and high sensitive fluorimetric method for the determination of carvedilol in medicine is developed. The measurement of relative fluorescence intensity was carried out at 356nm with excitation at 254nm. A linear relationship was obtained between the relative fluorescence intensity and concentration of carvedilol in the range of 0.50 to 270 ng/ml. The detection limit of this method is 0.19 ng/ml. This method can be used for determination of carvedilol in tablet samples. The results obtained by this method agreed with those by the official method.更多还原