高靈敏性氟離子熒光探針
發(fā)布時間:2018-08-02 21:27
【摘要】:香豆素類化合物因其多種優(yōu)良的特性,作為熒光探針已成為了研究熱點。氟離子是人體所必需的微量元素,適量的氟離子攝入有益于牙齒和骨骼的健康,過多或過少攝入氟離子都會對人體產(chǎn)生不良影響。因此,氟離子的檢測具有重大意義。本文選擇性的合成了以香豆素為母體的氟離子熒光探針。論文的主要內(nèi)容:(1)利用香豆素為母體,以叔丁基二甲基氯硅烷做為引入硅醚的試劑,合成了四個含有Si-O鍵的氟離子熒光探針化合物L(fēng)1、L2、L3、L4,其檢測機理是利用F和Si之間的強親和力,對Si-O鍵進行破壞,從而產(chǎn)生識別作用。產(chǎn)率分別為40%、45%、52%、48%。(2)利用香豆素為母體,綜合考慮了溶劑、催化劑、試劑、溫度、時間等條件,并選用對甲苯異氰酸酯為反應(yīng)試劑,合成了2個新型的以香豆素為母體的鈰離子熒光探針化合物L(fēng)5、L6。產(chǎn)率分別為90%、79%。(3)選擇化合物L(fēng)1作為探針分子,對其進行相關(guān)熒光性能的測試研究。研究發(fā)現(xiàn),探針L1分子在乙腈和水的比例為1:9的溶液中,探針L1分子對氟離子的檢測性能最佳,且其具有高靈敏性,其最低檢測限可以達到0.1μM 通過對比探針L1分子在不同pH條件紫外吸收和熒光發(fā)射光譜,發(fā)現(xiàn)其可適用在pH為2-10的范圍內(nèi),在此范圍內(nèi)較為穩(wěn)定適合用于檢測;在乙腈和水的比例為1:9的溶液中,通過加入Cl-,Br-,I-,CH_3COO-,HSO4-,H_2PO4-這6種陰離子作為干擾離子進行選擇性和抗干擾性檢測,發(fā)現(xiàn)探針L1分子對氟離子的檢測具有很高選擇性和抗干擾性,在這6種離子存在的情況下,對其檢測氟離子沒有任何有效性影響。(4)選擇化合物L(fēng)5作為探針分子,對其進行相關(guān)熒光性能的測試研究。研究發(fā)現(xiàn),探針L5分子在乙腈和水的比例為1:9的溶液中,探針L5分子對鈰離子的檢測性能最佳,且在其最低檢測限為0.1μM時仍具有較高靈敏性;通過對比探針L5分子在不同pH條件紫外吸收和熒光發(fā)射光譜,發(fā)現(xiàn)其可適用在pH為4-7的范圍內(nèi),在此范圍內(nèi)較為穩(wěn)定適合用于檢測;在乙腈和水的比例為1:9的溶液中,通過加入 Li+,Zn~(2+),Sr~(2+),Ni~(2+),Co~(2+),Ca~(2+),Fe~(2+),Hg~(2+),Ag+,Al~(3+),Cr~(3+),Fe~(3+),F-,Cl-,Br,I-,CH_3COO-,HSO4-,H_2PO4-這19種陰、陽離子進行選擇性和抗干擾性檢測,發(fā)現(xiàn)探針L5分子對鈰離子的檢測具有較高選擇性和抗干擾性,在這19種陰、陽離子存在的情況下,對其檢測鈰離子沒有任何有效性影響。
[Abstract]:Coumarin compounds as fluorescent probes have become a hot topic because of their many excellent properties. Fluoride ion is a necessary trace element in human body. Proper intake of fluoride ion is beneficial to the health of teeth and bones. Too much or too little fluoride ion intake will have adverse effects on human body. Therefore, the detection of fluorine ions is of great significance. Fluorine ion fluorescence probe with coumarin as parent was synthesized selectively in this paper. The main contents of this paper are as follows: (1) using coumarin as parent and tert Ding Ji dimethyl chlorosilane as the reagent of introducing silica ether, four fluorine fluorescent probe compounds L _ (1) L _ (2) and L _ (3) C _ (4) containing Si-O bond have been synthesized. The detection mechanism is to utilize the strong affinity between F and Si. The Si-O key is broken to produce recognition. The yields were 40% and 45%, respectively. (2) the solvent, catalyst, reagent, temperature, time and so on were taken into account with coumarin as the parent, and p-toluene isocyanate was selected as the reaction reagent. Two novel cerium ion fluorescent probe compounds L _ 5N _ L _ 6 with coumarin as parent were synthesized. The yields were 90 and 79 respectively. (3) compound L1 was selected as probe molecule and its fluorescence properties were tested. It was found that the probe L1 molecule had the best detection performance for fluorine ion in the solution with the ratio of acetonitrile to water at 1:9, and the probe L1 molecule had high sensitivity. The lowest detection limit can reach 0.1 渭 M. By comparing the UV absorption and fluorescence emission spectra of the probe L1 at different pH conditions, it is found that it can be used in the range of pH 2-10, and it is more stable and suitable for detection in this range. In a solution with the ratio of acetonitrile to water at 1:9, the selective and anti-interference properties of the probe L1 molecule for fluorine ion detection were found to be highly selective and anti-interference by adding Cl-nil Br-tir I-Che CH3COO-HSO4-H2PO4- these six kinds of anions as interference ions. In the presence of these six ions, there was no effect on the detection of fluorine ions. (4) the related fluorescence properties of L5 as probe molecule were studied. It is found that the probe L5 has the best detection performance for cerium ion in the solution with the ratio of acetonitrile to water at 1:9, and still has a high sensitivity when the detection limit is 0.1 渭 M. By comparing the UV absorption and fluorescence emission spectra of the probe L5 at different pH conditions, it is found that the probe can be applied in the range of pH 4-7, and is stable and suitable for detection in the solution with the ratio of acetonitrile to water at 1:9. By adding Li Li Zn ~ (2) O _ (2) Sr ~ (2) O _ (2) Co ~ (2) Co ~ (2) O _ (2) Fe ~ (2) O _ (2) H _ g ~ (2) O _ (2) Hg ~ (2) O _ (2) O _ (3) Cr ~ (3) O _ (3) Fe ~ (3) O _ (3) Fe ~ (3) O _ (3) Fe ~ (3) O _ (3) -Fe ~ (3) O _ (3) -Fe ~ (3) O _ (3) F ~ (2) O ~ (3) O _ (3) -BrI-CH3COO-HSO _ 4-H2PO _ (4), 19 anion, cations were tested for selectivity and anti-interference of cerium ion. In the presence of cations, there is no effect on the detection of cerium ions.
【學(xué)位授予單位】:東華大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2017
【分類號】:O657.3
本文編號:2160785
[Abstract]:Coumarin compounds as fluorescent probes have become a hot topic because of their many excellent properties. Fluoride ion is a necessary trace element in human body. Proper intake of fluoride ion is beneficial to the health of teeth and bones. Too much or too little fluoride ion intake will have adverse effects on human body. Therefore, the detection of fluorine ions is of great significance. Fluorine ion fluorescence probe with coumarin as parent was synthesized selectively in this paper. The main contents of this paper are as follows: (1) using coumarin as parent and tert Ding Ji dimethyl chlorosilane as the reagent of introducing silica ether, four fluorine fluorescent probe compounds L _ (1) L _ (2) and L _ (3) C _ (4) containing Si-O bond have been synthesized. The detection mechanism is to utilize the strong affinity between F and Si. The Si-O key is broken to produce recognition. The yields were 40% and 45%, respectively. (2) the solvent, catalyst, reagent, temperature, time and so on were taken into account with coumarin as the parent, and p-toluene isocyanate was selected as the reaction reagent. Two novel cerium ion fluorescent probe compounds L _ 5N _ L _ 6 with coumarin as parent were synthesized. The yields were 90 and 79 respectively. (3) compound L1 was selected as probe molecule and its fluorescence properties were tested. It was found that the probe L1 molecule had the best detection performance for fluorine ion in the solution with the ratio of acetonitrile to water at 1:9, and the probe L1 molecule had high sensitivity. The lowest detection limit can reach 0.1 渭 M. By comparing the UV absorption and fluorescence emission spectra of the probe L1 at different pH conditions, it is found that it can be used in the range of pH 2-10, and it is more stable and suitable for detection in this range. In a solution with the ratio of acetonitrile to water at 1:9, the selective and anti-interference properties of the probe L1 molecule for fluorine ion detection were found to be highly selective and anti-interference by adding Cl-nil Br-tir I-Che CH3COO-HSO4-H2PO4- these six kinds of anions as interference ions. In the presence of these six ions, there was no effect on the detection of fluorine ions. (4) the related fluorescence properties of L5 as probe molecule were studied. It is found that the probe L5 has the best detection performance for cerium ion in the solution with the ratio of acetonitrile to water at 1:9, and still has a high sensitivity when the detection limit is 0.1 渭 M. By comparing the UV absorption and fluorescence emission spectra of the probe L5 at different pH conditions, it is found that the probe can be applied in the range of pH 4-7, and is stable and suitable for detection in the solution with the ratio of acetonitrile to water at 1:9. By adding Li Li Zn ~ (2) O _ (2) Sr ~ (2) O _ (2) Co ~ (2) Co ~ (2) O _ (2) Fe ~ (2) O _ (2) H _ g ~ (2) O _ (2) Hg ~ (2) O _ (2) O _ (3) Cr ~ (3) O _ (3) Fe ~ (3) O _ (3) Fe ~ (3) O _ (3) Fe ~ (3) O _ (3) -Fe ~ (3) O _ (3) -Fe ~ (3) O _ (3) F ~ (2) O ~ (3) O _ (3) -BrI-CH3COO-HSO _ 4-H2PO _ (4), 19 anion, cations were tested for selectivity and anti-interference of cerium ion. In the presence of cations, there is no effect on the detection of cerium ions.
【學(xué)位授予單位】:東華大學(xué)
【學(xué)位級別】:碩士
【學(xué)位授予年份】:2017
【分類號】:O657.3
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