分析条件对薄层色谱法测定TPPCo纯度的影响研究.docVIP

摘 要 卟啉及其金属配合物是一类具有刚性大环共轭体系的分子。目前，这类化合物表征鉴定手段主要是采用一些大型分析仪器。这些方法不便于TPPCo及其配合物及应用过程中的跟踪、监测。 本论文的目的是建立一种方便、快捷的TPPCo分离分析方法，以便于为TPPCo合成应用过程中提供有效的跟踪检测方法。 本课题采用条件实验法，研究了展开剂种类、极性、薄层厚度、活化时间等因素对TPPCo分离行为的影响，获得适宜分离展开条件后采用薄层色谱扫描仪，考察了TPPCo定量测定的线性范围、精密度、检出限。 实验结果表明：浓度为0.048μg/μL的TPPCo在薄层板厚度0.3mm，活化时间为60min，展开体系为环己烷:乙酸乙酯:甲醇（体积比为12:4:6）时，分离效果最好，斑点均不拖尾，Rf为0.5，适于定量分析。（1）当薄层板厚度变大（0.25-0.35mm），样品斑点的比移值变小；（2）展开剂极性变大，样品斑点的比移值变大；（3）薄层板活化时间延长，样品斑点的比移值先变大后变小。 TPPCo薄层扫描定量测定的线性范围0.048μg-0.384μg，标准方程：Y=2193.33X+131.6（r=0.9998），RSD=7.41%，测定准确度仅为87.5%。 关键词：薄层色谱；四苯基钴卟啉；卟啉 Abstract Porphyrins and their metal complexes are a class of molecules with a rigid macrocyclic conjugated system. At present, they are characterized mainly by some large analytical instruments.These methods is not convenient to monitor for TPPCo and its complexes in applications. The purpose of this paper is to establish a convenient, fast methods for separation and analysis of TPPCo, to provide effective tracking testing methods for TPPCo in the process applications . In experiments, the effects of developing solvent type, polarity, layer thickness and activation time of thin layer on TPPCo separation behavior were studied by conditional experiment methods,and obtained the appropriate separation conditions.Under appropriate separation conditions,linear range,precision,and RSD for determination of TPPCo quantitative were examined by TLC scanner. The experimental results show that: the concentration of 0.048μg/μL TPPCo in thin layer plate thickness of 0.3mm, activation time for 60min, a system for the cyclohexane: ethyl acetate: methanol (volume ratio of 12:4:6), separation effect is best, spots are not trailing，Rf=0.5,is suitable for quantitative determination.（1）Rf value decreases with the thickness of the thin layer plate increases (0.25-0.35mm);（2）Rf value increases with developing solvent polarity increases;（3）Rf value first increases then decreases with thin layer plate activation time extends. The quantitative dete