本文關(guān)鍵詞：小分子熒光探針的合成及其在羥基自由基和汞離子檢測中的應(yīng)用　出處：《山東農(nóng)業(yè)大學(xué)》2012年碩士論文　論文類型：學(xué)位論文

  更多相關(guān)文章： ·OH 香草醛縮苯胺 熒光猝滅 羅丹明B酰肼-肉桂酸硫脲 硫代羅丹明B-水楊醛酰腙 Hg~(2+)

【摘要】：活性氧粒子（ROS）不斷產(chǎn)生于有機(jī)體的氧化代謝過程，它是誘發(fā)細(xì)胞損傷和老化重要的因素。過量活性氧和其衍生物的存在，可誘發(fā)許多疾病的產(chǎn)生。因此，ROS的檢測得到了極大關(guān)注。羥基自由基（·OH）是最具有代表性的自由基。迄今為止,檢測和清除羥基自由基方法已有許多，其中熒光分析由于具有靈敏度高、選擇性好、操作簡單等優(yōu)勢受到人們的青睞。但由于用于檢測·OH的熒光探針比較少見，因此開發(fā),對·OH專一識(shí)別、快速響應(yīng)的熒光探針已成為研究的熱點(diǎn)。 汞是一種毒性較強(qiáng)的金屬元素且嚴(yán)重危害人類的健康，因此開發(fā)具有選擇性、靈敏度高、選擇性強(qiáng)、水溶性好的探針，已成為熒光法測定Hg~(2+)的焦點(diǎn)。羅丹明類熒光染料由于具有摩爾消光系數(shù)高、光穩(wěn)定性好、熒光量子產(chǎn)率高、有較長的激發(fā)波長和發(fā)射波長等優(yōu)異的光物理和光化學(xué)性能，因此拓展羅丹明類染料作為熒光探針在Hg~(2+)熒光測定中的應(yīng)用十分必要。 本文合成了三種新型熒光探針，，利用探針對·OH和Hg~(2+)進(jìn)行了檢測，提出了新的檢測方法，主要研究工作： (1)合成了熒光探針香草醛縮苯胺，利用紅外光譜、元素分析、核磁等方法對探針結(jié)構(gòu)進(jìn)行了表征；該探針的熒光可被·OH猝滅，藕合Fenton反應(yīng)，建立了一種熒光猝滅法測定·OH的新方法，該方法的檢測線性范圍為2×10~(-6)-2×10~(-5)mol·L~(-1)，檢出限為8×10~(-7)mol·L~(-1)。利用該方法測定了幾種大豆提取液對·OH清除作用，結(jié)果滿意。 (2)合成了一種新的RBHT（羅丹明B酰肼-肉桂酸硫脲)熒光探針，利用紅外光譜、元素分析、核磁等方法對探針結(jié)構(gòu)進(jìn)行了表征；該探針與Hg~(2+)結(jié)合后產(chǎn)生較強(qiáng)熒光，由此建立了一種測定汞的熒光法分析方法。Hg~(2+)測定的線性范圍為8.0×10~(-7)~(-6).0×10~(-6)mol·L~(-1)，檢出限為7.0×10~(-8)mol·L~(-1)。該方法具有操作簡單、靈敏度高和選擇性好等特點(diǎn)。方法試用于自來水、河水中痕量汞的測定，結(jié)果滿意。 (3)根據(jù)Hg~(2+)具有很強(qiáng)的嗜硫性特點(diǎn)，設(shè)計(jì)并合成了探針硫代羅丹明B-水楊醛酰腙。利用紅外光譜、元素分析、核磁等方法對探針結(jié)構(gòu)進(jìn)行了表征；該化合物可以有效地與Hg~(2+)絡(luò)合，使羅丹明的環(huán)狀結(jié)構(gòu)被破壞，生成開環(huán)化合物。Hg~(2+)與探針分子相結(jié)合，溶液由無色、無熒光，到溶液變?yōu)樽霞t色，產(chǎn)生強(qiáng)烈的熒光。該化合物在Hg~(2+)濃度為1.0×10~(-8)~(-1).0×10~(-6)mol·L~(-1)范圍內(nèi)，有很好的線性。檢出限為5.4×10~(-9)mol·L~(-1)。方法成功用于自來水、河水中Hg~(2+)的檢測，結(jié)果滿意。
[Abstract]:Reactive oxygen species (Ros) are produced by the oxidative metabolism of organisms, which are important factors in inducing cell damage and aging, and the presence of excess reactive oxygen species and its derivatives. It can induce many diseases. Therefore, the detection of Ros has attracted much attention. Hydroxyl radical (路OH) is the most representative free radical. So far. There are many methods for detecting and scavenging hydroxyl radicals, among which fluorescence analysis has high sensitivity and selectivity. The advantages of simple operation are favored by people, but the fluorescence probe used for the detection of 路OH is rare, so it has become a hot research topic to develop a fluorescence probe that specifically recognizes 路OH and responds quickly. Mercury is a highly toxic metal element and seriously endangers human health. Therefore, it has high selectivity, high sensitivity, high selectivity and good water solubility. Rhodamine fluorescent dyes have high molar extinction coefficient, good light stability and high fluorescence quantum yield. It is necessary to expand the application of Rhodamine dyes as a fluorescent probe in the determination of Hg~(2 fluorescence because of their excellent photophysical and photochemical properties such as long excitation wavelength and emission wavelength. In this paper, three new fluorescent probes were synthesized, and the 路OH and Hg~(2 were detected by the probes. A new detection method was proposed, and the main research work was as follows: The fluorescence probe vanillin aniline was synthesized. The structure of the probe was characterized by IR, elemental analysis and NMR. The fluorescence of the probe can be quenched by 路OH and coupled with Fenton reaction. A new method for the determination of 路OH by fluorescence quenching method has been established. The linear range of this method is 2 脳 10 ~ (-6) ~ (-2) 脳 10 ~ (10) ~ (-5) mol 路L ~ (-1). The detection limit was 8 脳 10 ~ (10) ~ (-7) mol 路L ~ (-1) 路L ~ (-1). The method was used to determine the scavenging effect of several soybean extracts on 路OH with satisfactory results. A novel RBHT (Rhodamine B hydrazide-thiourea cinnamate) fluorescence probe was synthesized and characterized by IR, elemental analysis and NMR. The probe combines with Hg~(2 to produce strong fluorescence. A fluorescence method for the determination of mercury was established. The linear range of determination was 8.0 脳 10 ~ (10) ~ (-7) ~ (?) ~ (6). 0 脳 10 ~ (10) ~ (-6) mol 路L ~ (-1). . The detection limit is 7.0 脳 10 ~ (10) ~ (-8) mol 路L ~ (-1) 路L ~ (-1). The method has the advantages of simple operation, high sensitivity and good selectivity. The method has been applied to the determination of trace mercury in tap water and river water. The result is satisfactory. (3) according to the characteristic of Hg~(2, the probe thiorhodamine B- salicylaldehyde-acyl Hydrazone was designed and synthesized. Infrared spectrum and elemental analysis were used. The structure of the probe was characterized by NMR. The compound can be efficiently complexed with Hg~(2), resulting in the destruction of the ring structure of Rhodamine and the formation of ring-opening compound. Until the solution turns purple. Strong fluorescence was produced. The concentration of the compound was 1.0 脳 10 ~ (10) ~ (-8) ~ (-1) ~ (-1). 0 脳 10 ~ (10) ~ (-1) mol 路L ~ (-1). The detection limit is 5.4 脳 10 ~ (-9) mol 路L ~ (-1). The method has been successfully applied to the determination of Hg~(2 in tap water and river water with satisfactory results.
【學(xué)位授予單位】：山東農(nóng)業(yè)大學(xué)
【學(xué)位級(jí)別】：碩士
【學(xué)位授予年份】：2012
【分類號(hào)】：R115;O657.3

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