本文選題：加替沙星 + 氧氟沙星　； 參考：《寧夏大學》2017年碩士論文

【摘要】：本論文分別以氟喹諾酮類抗生素中的加替沙星(GTFX)和氧氟沙星(OFLX)為模板分子,制得了 4種分子印跡聚合物。利用紫外分光光度計對分子印跡聚合物的吸附性能進行了詳細考察。將其作為吸附劑,結合高效液相色譜(HPLC)分析,可用于牛奶、湖水、牛血清樣品中GTFX、OFLX的分離富集與分析測定。主要工作如下:1.在甲醇-乙腈(1:1,V/V)混合溶液中,基于單分散交聯(lián)聚甲基丙烯酸環(huán)氧丙酯(PGMA/EDMA)微球,以GTFX為模板分子,甲基丙烯酸(MAA)為功能單體,制得加替沙星表面分子印跡聚合物(MIP/GMA/EDMA)。利用紫外分光光度計研究了 GTFX與MAA的相互作用。通過靜態(tài)吸附實驗考察了MIP/PGMA/EDMA對GTFX的吸附容量和選擇性吸附能力,利用Scathard曲線計算了最大表觀吸附量和離解常數(shù);通過動態(tài)吸附實驗考察了 MIP/PGMA/EDMA對GTFX的吸附速率,利用動力學方程分析了其動力學行為。將該MIP/PGMA/EDMA制成分子印跡固相萃取(MIP-SPE)柱,考察其重復使用性能。結合HPLC分析,建立了一種分離、檢測牛奶和湖水中GTFX的方法。2.采用共沉淀法合成Fe3O4納米粒子,利用溶膠-凝膠技術在Fe3O4表面包覆SiO2,隨后引入雙鍵得到Fe3O4@SiO2-MPS。以此為載體,GTFX為模板分子,制得加替沙星磁性表面分子印跡聚合物(M-MIPs)。用透射電鏡(TEM)、X射線衍射分析(XRD)、磁化強度分析(VSM)等手段對各步磁性粒子進行了表征。通過吸附實驗考察了 M-MIPs對GTFX的吸附性能。將該M-MIPs作為吸附劑,結合HPLC分析,用于分離、檢測牛奶中的GTFX。3.利用紫外分光光度計分析模板分子OFLX與兩種功能單體MAA和4-乙烯基吡啶(4-VP)的結合情況,確定了最佳功能單體;選取OFLX與最佳功能單體的摩爾比為1:4、1:6、1:8和1:10,分別制備印跡聚合物和非印跡聚合物,通過對比吸附量和印跡因子,確定了最佳制備比例。采用沉淀聚合法,以50 mL甲醇-水(9:1,V/V)混合溶液為溶劑,制得氧氟沙星限進介質分子印跡聚合物(RAM-MIPs)。選取GTFX、恩諾沙星(ENRO)和磺胺甲基嘧啶(SMR)作為競爭分子,考察了 RAM-MIPs對OFLX的選擇性吸附性能。選取牛血清白蛋白(BSA)作為模型蛋白,考察了 RAM-MIPs對蛋白質大分子的排阻能力。將該RAM-MIPs制成MIP-SPE柱,考察其循環(huán)使用性能;與HPLC聯(lián)用,用于凈化、萃取和檢測牛奶中的OFLX。4.以5.0 μm硅膠為載體,OFLX為模板分子,MAA為功能單體,甲基丙烯酸縮水甘油酯(GMA)為親水性功能單體,采用表面原子轉移自由基技術(SI-ATRP),制得硅膠表面氧氟沙星限進介質分子印跡聚合物(Sil-RAM-MIPs)。利用Scatchard模型評價Sil-RAM-MIPs對OFLX的結合特性;利用Langmuir和Freundlich等溫模型分析Sil-RAM-MIPs對OFLX的吸附行為。結合固相萃取技術,考察了 Sil-RAM-MIPs對BSA的排阻效果,并將其用于分析牛血清樣品中的OFLX。
[Abstract]:In this paper, four molecularly imprinted polymers were prepared using gatifloxacin (GTFX) and ofloxacin (OFLX) as template molecules in fluoroquinolones. The adsorption properties of molecularly imprinted polymers were investigated by UV spectrophotometer. It can be used for the separation, enrichment and determination of GTFX OFLX in milk, lake water and bovine serum samples by high performance liquid chromatography (HPLC). The main work is as follows: 1. In methanol-acetonitrile (1: 1 / 1 V / V) solution, a molecularly imprinted polymer (MIP / GMA / EDMAA) on the surface of gatifloxacin was prepared on the basis of monodisperse crosslinked poly (propyl methacrylate) (PGMA / EDMA) microspheres, using GTFX as template molecule and MAA as functional monomer. The interaction between GTFX and MAA was studied by UV spectrophotometer. The adsorption capacity and selective adsorption capacity of MIP/PGMA/EDMA to GTFX were investigated by static adsorption experiment, the maximum apparent adsorption capacity and dissociation constant were calculated by Scathard curve, and the adsorption rate of MIP/PGMA/EDMA on GTFX was investigated by dynamic adsorption experiment. The dynamic behavior is analyzed by using the kinetic equation. The MIP-SPE column was prepared by molecularly imprinted solid phase extraction (MIP-SPE). A method for the separation and detection of GTFX in milk and lake water was established by HPLC analysis. Fe3O4 nanoparticles were synthesized by coprecipitation method. Sio _ 2 was coated on the surface of Fe3O4 by sol-gel technique, and then Fe _ 3O _ 4 @ Sio _ 2-MPS was obtained by introducing double bonds. The gatifloxacin magnetic surface molecularly imprinted polymer (M-MIPsN) was prepared by using GTFX as the template molecule. The magnetic particles were characterized by means of transmission electron microscopy (TEM) and X-ray diffraction (XRD), and magnetization analysis (VSM). The adsorption properties of M-MIPs to GTFX were investigated by adsorption experiments. The M-MIPs was used as an adsorbent for the separation and detection of GTFX. 3. 3 in milk by HPLC analysis. The combination of template molecule OFLX with two functional monomers MAA and 4-vinylpyridine 4-VPwas analyzed by UV spectrophotometer and the best functional monomer was determined. The molar ratio of OFLX to the best functional monomer was 1: 4: 1: 6: 8 and 1: 10, respectively. The imprinted polymer and non-imprinted polymer were prepared respectively. The optimum preparation ratio was determined by comparing the adsorption amount and the imprinting factor. A molecular imprinted polymer (RAM-MIPsN) of ofloxacin was prepared by precipitation polymerization with 50 mL methanol-water (9: 1 V / V) mixed solution as solvent. GTFX, enrofloxacin enro and sulfamethylpyrimidine (SMR) were selected as competitive molecules to investigate the selective adsorption of OFLX by RAM-MIPs. Bovine Serum Albumin (BSA) was selected as model protein to investigate the resistance of RAM-MIPs to protein macromolecules. The RAM-MIPs was prepared into a MIP-SPE column to investigate its recycling performance, and was combined with HPLC for purification, extraction and detection of OFLX. 4 in milk. Using 5.0 渭 m silica gel as carrier, OFLX as functional monomer, glycidyl methacrylate (GMAA) as hydrophilic functional monomer, surface atom transfer radical technique was used to prepare silica gel surface ofloxacin molecular imprinted polymer, Sil-RAM-MIPs. Scatchard model was used to evaluate the binding characteristics of Sil-RAM-MIPs to OFLX, and Langmuir and Freundlich isothermal models were used to analyze the adsorption behavior of Sil-RAM-MIPs to OFLX. Combined with solid phase extraction (SPE) technique, the inhibition effect of Sil-RAM-MIPs on BSA was investigated and used for the analysis of OFLX in bovine serum samples.
【學位授予單位】：寧夏大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O631.3;O652

【參考文獻】

中國期刊全文數(shù)據(jù)庫 前10條

1 馬潤恬;師彥平;;樣品分析中分子印跡固相萃取的新技術進展[J];色譜;2016年03期

2 焦文君;;氟喹諾酮類藥物的藥理特點及研究進展[J];中國實用醫(yī)藥;2015年32期

3 鄭鵬磊;羅智敏;暢瑞苗;葛燕輝;杜瑋;常春;傅強;;青霉噻唑酸表面分子印跡聚合物的制備及其吸附性能的考察[J];色譜;2015年09期

4 陳思遠;董旭;查劉生;;表面引發(fā)原子轉移自由基聚合法合成無機/有機核殼復合納米粒子[J];化學進展;2015年07期

5 叢姣姣;羅靜;高雅涵;劉曉亞;;表面分子印跡研究進展[J];高分子通報;2015年05期

6 趙冬艷;喬旭光;徐志祥;;殼聚糖在分子印跡技術中的應用研究進展[J];食品與生物技術學報;2014年06期

7 王茹娟;馬應霞;路翠萍;李濤;杜雪巖;;谷胱甘肽磁性分子印跡聚合物的制備及吸附性能研究[J];化學學報;2014年05期

8 夏英;張瀾;趙爾成;賈春虹;朱曉丹;;煙嘧磺隆分子印跡微球的制備及其吸附性能的考察[J];色譜;2014年02期

9 何世偉;黃忠平;朱巖;;新型碳納米管色譜固定相制備的研究進展[J];色譜;2013年12期

10 李金花;溫瑩瑩;陳令新;;分子印跡聚合物固相萃取研究進展[J];色譜;2013年03期

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