【正文】
I 摘 要 卟啉及其金屬配合物是一類具有剛性大環(huán)共軛體系的分子。目前,這類化合物表征鑒定手段主要是采用一些大型分析儀器。這些方法不便于 TPPCo 及其配合物及應(yīng)用過程中的跟蹤、監(jiān)測(cè)。 本論文的目的是建立一種方便、快捷的 TPPCo 分離分析方法,以便于為TPPCo 合成應(yīng)用過程中提供有效的跟蹤檢測(cè)方法。 本課題采用條件實(shí)驗(yàn)法,研究了展開劑種類、極性、薄層厚度、活化時(shí)間等因素對(duì) TPPCo 分離行為的影響,獲得適宜分離展開條件后采用薄層色譜掃描儀,考察了 TPPCo 定量測(cè)定的線性范圍、精密度、檢出限。 實(shí)驗(yàn)結(jié)果表 明:濃度為 ,活化時(shí)間為 60min,展開體系為 環(huán)己烷 :乙酸乙酯 :甲醇(體積比為 12:4:6)時(shí),分離效果最好,斑點(diǎn)均不拖尾, Rf 為 ,適于定量分析。 ( 1)當(dāng)薄層板厚度變大( ),樣品斑點(diǎn)的比移值變??;( 2)展開劑極性變大,樣品斑點(diǎn)的比移值變大;( 3)薄層板活化時(shí)間延長,樣品斑點(diǎn)的比移值先變大后變小。 TPPCo 薄層掃描定量測(cè)定的線性范圍 ,標(biāo)準(zhǔn)方程:Y=+( r=), RSD=%,測(cè)定準(zhǔn)確度僅為 %。 關(guān)鍵詞:薄層色譜;四苯基鈷卟啉;卟啉 II Abstract Porphyrins and their metal plexes are a class of molecules with a rigid macrocyclic conjugated system. At present, they are characterized mainly by some large analytical methods is not convenient to monitor for TPPCo and its plexes 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 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 thin layer plate thickness of , 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=,is suitable for quantitative determination.( 1) Rf value decreases with the thickness of the thin layer plate increases ()。( 2) 錯(cuò)誤 !未找到引用源。 developing solvent polarity increases。( 3) Rf value first increases then decreases with thin layer plate activation time extends. The quantitative determination of linear range of TPPCo is by thin layer scanning, standard equation: Y=+ (r=), RSD=%, the measuring accuracy is only %. Key words:thinlayer chromatography。tetraphenylporphyrin cobalt。porphyrin III 目 錄 摘 要 ..........................................................................................................................I Abstract........................................................................................................................ II 第 1章 引 言 ............................................................................................................. 1 卟啉概述 .......................................................................................................... 1 卟啉及金屬卟啉的結(jié)構(gòu)性質(zhì) ................................................................ 1 卟啉及金屬卟啉化合物的合成 ............................................................ 1 卟啉及金屬卟啉的應(yīng)用 ........................................................................ 1 卟啉及金屬卟啉的發(fā)展現(xiàn)狀與趨勢(shì) .................................................... 1 薄層色譜法 ...................................................................................................... 2 薄層色譜類型 ........................................................................................ 2 薄層掃描法及定量分析 ........................................................................ 2 薄層色譜檢測(cè)方法及應(yīng)用 ................................................................... 3 課題的目的和意義 .......................................................................................... 3 課題的目的 ............................................................................................ 3 課題的意義 ............................................................................................ 4 第 2章 實(shí)驗(yàn)部分 ......................................................................................................... 5 實(shí)驗(yàn)所需藥品、試劑 ..................................................................................... 5 主要儀器、設(shè)備 .............................................................................................. 6 實(shí)驗(yàn)原理