分光光度法在药物分析中的应用——银杏黄酮、烟酰胺的分析方法研究

【作者】 上官小东；

【导师】 郎惠云；

【作者基本信息】 西北大学 ， 分析化学， 2003， 硕士

【摘要】 本文研究了分光光度法和原子吸收光谱法测定烟酰胺、羟甲基烟酰胺及银杏黄酮的分析方法，提出了银杏黄酮的三种测定方法和烟酰胺及羟甲基烟酰胺的测定新方法，并应用于实际样品的测定，获得满意结果。本文由以下六章组成： 第一章：综述。对紫外-可见分光光度法和原子吸收光谱法在药物分析中的应用进行了文献综述。 第二章：高铁盐配位-分光光度法测定药物制剂中烟酰胺含量。本文首次提出了测定烟酰胺含量的新方法，它是基于在碱性介质中烟酰胺与羟胺反应生成异羟肟酸，反应产物与Fe³⁺反应生成紫红色络合物，在496nm波长处有最大吸收，其络合比为3：1。该方法的线性范围为10.0～200.0 μg／mL，相关系数为0.9997，表观摩尔吸光系数ε=5.11×10⁴ L·mol^-1·cm^-1，平均回收率为101.2％。用于烟酰胺片剂含量的测定，具有灵敏度高、线性范围宽等优点。 第三章：高锰酸钾氧化-分光光度法测定羟甲基烟酰胺含量。首次提出了测定羟甲基烟酰胺的新方法，它是利用羟甲基烟酰胺中存在的羟基，可以被酸性高锰酸钾氧化而使其溶液变色。根据高锰酸钾溶液的吸光度来测定羟甲基烟酰胺的含量。该方法的线性范围为2.0～40.0μg／mL，相关系数为0.9994，摩尔吸光系数为1.80×10⁴ L·mol^-1·om^-1，平均回收率为100.5％。用于实际样品的测定，结果满意。 第四章：间接原子吸收法测定银杏黄酮含量。首次提出了间接测定银杏叶精提物中银杏黄酮的原子吸收光谱法。它是基于银杏黄酮能与乙酸铅发生配合反应，生成难溶的棕黄色沉淀，经离心分离后，用原子吸收法测定上清液中过量的铅离子，可间接测定银杏黄酮的含量。方法线性范围为5.0～30.0 μg／mL，RSD为1.7％，回收率为98.0～100.3％。 第五章：氯化铝-分光光度法测定银杏黄酮含量。首次提出了三氯化铝-分光光度法测定药物制剂中银杏黄酮含量的新方法。该法是基于银杏黄酮能与氯化铝反应生成黄色络合物，此物质在408nm处有最大吸收。方法的线性范围为2.0～110.0μg／mL，r=0.9999，回收率为99.7～100.8％。用于银杏黄酮片剂含量的测分光光度法在药物分析中的应用中文摘要定，获得结果满意。 第六章:钨酸钠一分光光度法测定银杏黄酮含量。首次提出了钨酸钠一分光光度法测定药物制剂中银杏黄酮含量的新方法。该法是基于银杏黄酮能与钨酸钠反应生成黄色钨酸醋，该物质在304nm处有最大吸收。该方法的线性范围为4.0一90.0p创山工，间.9998，回收率为100.份100.60/0。用于实际样品的测定，获得结果满意。更多还原

【Abstract】 This thesis studies the analytical methods of determination of Nicotinamide, N-hydroxymethylnicotinamide and flavonoids of Ginkgo biloba by Ultraviolet-visible Spectrophotometry and Atomic Absorption Spectroscopy. Three determinate methods of flavonoids of Ginkgo biloba and a new method of Nicotinamide and N-hydroxymethylnicotinamide by Ultraviolet Spectrophotometry are reported .The methods had been applied to determine the samples and obtained satisfactory results. It includes six parts as follows:Part I : Review. A review of the application of Ultraviolet-visible Spectrophotometry and Atomic Absorption Spectroscopy in Pharmaceuticals is given.Part II: Spectrophotometry of Nicotinamide by Coordination reaction of Ferric Chloride. A new method of spectrophotomertry of Nicotinamide by coordination reaction of Ferric chloride was studied. This basis is that the acetamido group of Nicotinamide could react with hydroxylamine to form N-hydroxylamine-amide, which gives color reaction with Fe3+ and could be used determination of Nicotinamide by spectrophotometry at the wavelength of 496nm. The linear region was 10.0~200.0 u g/mL, r=0.9997, e =5.11 X104 L mol-1 cm-1, RSD=1.2%,the average recovery was 101.2% .Part III: Determination of N-hydroxymethylnicotinamide by Potassium permanganate oxidation. A new method of Determination of N-hydroxymethylnicotinamide by Potassium permanganate oxidation was studied. The hydroxy group of N-hydroxymethylnicotinamide could react with Potassium permanganate, which reduced color of Potassium permanganate and was used determination of N-hydroxymethylnicotinamide by spectrophotometry at the wavelength of 526nm. The linear region was 2.0~40.0 ug/mL, r=0.9994, e =1.80X 104L mol-1 cm-1, the average recovery was 100.5%.Part IV: Indirect Determination of flavonoids of Ginkgo biloba.by AtomicAbsorption Spectroscopy. An atomic absorption spectroscopy was used for indirect determination of flavonoids of Ginkgo biloba via pb (II) precipitate. In the method, the flavonoids of Ginkgo biloba reacted with pb2+ and led to brown-yellow precipitate. The precipitate is centrifuged to subside. The pb2+ in supernatant is determined by AAS. The calibration curve was linear for flavonoids of Ginkgo biloba in the range of 5.0 ~ 30.0 v. g/mL, r=0.9995, RSD=1.7% and the recovery is 98.0-100.3%(n=10).Part V : Determination of flavonoids of Ginkgo biloba by aluminum chloride spectrophotometry. A new method for determining of flavonoids of Ginkgo biloba by aluminum chloride spectrphotometry was studied. The basis is that flavonoids of Ginkgo biloba could react with aluminum chloride. The linear region was 2.0~ 110.0 u g/mL, r=0.9999, and the recovery was 99.7-100.8%.Part VI: Determination of flavonoids of Ginkgo biloba by sodium tungstate spectrophotometry. A new method for determining of flavonoids of Ginkgo biloba by sodium tungstate spectrphotometry was studied. It based on which flavonoids of Ginkgo biloba could react with sodium tungstate to form yellow ester tungstate. The linear region was 4.0~90.0 u g/mL,R2=0.9997, and the recovery was 100-100.6%.更多还原