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Preparation Of Fullerene Derivatives And Its Application In Capillary Electrophoresis

Posted on:2017-01-11Degree:MasterType:Thesis
Country:ChinaCandidate:Q ShuFull Text:PDF
GTID:2131330503486043Subject:Analytical Chemistry
Abstract/Summary:PDF Full Text Request
Fullerene is the third allotrope of carbon which was discovered in the 1980s, it has a unique spherical structure, which structure is similar to football, and itwas well-known as football-ene, it has been extensively studied in the fields of materials science, analytical science and bio-medicine because of its unique spherical structure and attractive physical and chemical properties. The endohedral metallofullerene is one of the fullerene family, and it has some unique properties which different from hollow fullerenes as it embedded the metal in the carbon cage. And the preparation and functional modification of the metallofullerene are still the hot-pot in the fullerene research.The thesis can be divided into three parts:1. The yttrium endohedral metallofullerene was synthesized by the same DC arc discharge method, and the metallofullerene was selective extracted by N, N-dimethylformamide. After multi-step separations, combined the HPLC with mass spectrometry, we got two isomers of the Y@C82 which were high purity. The UV-visible-near infrared absorption spectra were investigated to study the carbon cage symmetry of these two isomers, combined with the reported literature, we preliminary judged these two isomer as C2v and Cs, wherein Cs isomer has not yet been reported.2. In order to explore the chemical properties of the Y@Cs2 isomer which has never been reported. The high purity Y@Cs-C82 was reacted with bromo diethylmalonate based on the Bingel-Hirsch reaction. Then the products which have been purified were characterized by the mass spectrometry and visible-near infrared spectroscopy, at last, we get the structure of one mono-adduct product by the single crystal XRD. This work has an important significance in the analysis of the structure and chemical properties of Y@C82.3. The fullerene (C60) was prepared by the DC arc discharge method, and a water-soluble fullerene (C60CH-COOH) was synthesized though the carboxyl derivatized reaction. Then a water-soluble photosensitive material diazoresin (DR) regards as a connection reagent, using the self-assembled layer by layer (LBL) technique, to establish a covalent bond of DR/C60CH-COOH coating on the capillary wall. Then the capillary coating column was used for the separation of protein in the capillary electrophoresis, and it can achieve baseline separation when separates four kinds of protein, and it shows good reproducibility and good stability.In this paper, the yttrium metallofullerene were studied by preparetion, isolation and chemically modified. It was found that the embedded of the the metal yttrium improved the chemical activity of carbon atom in the carbon cage.This paper explored the chemical properties of Y@Cs-C82 for the first time, and got the structure of one mono-adduct, it has positive significance in the depth study of the chemical activity as well as the design and synthesis of novel functional molecules of the metallofullerenes.In this paper, the functional carbon material C60CH-COOH was modified in the capillary wall, the unique spherical structure of C60 effectively reduced the exposure of proteins with the capillary wall silanols, and improve the lubricity ability of the coating, and effectively improve the separation efficiency of proteins, shorten the separation time.
Keywords/Search Tags:water-soluble fullerene, capillary coating fabrication, protein separation, endohedral metallofullerene, chemical modification
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