發(fā)布時間：2018-05-13 14:37

  本文選題：磁性分子印跡聚合物 + 虛擬模板��； 參考：《中國科學(xué)技術(shù)大學(xué)》2017年碩士論文

【摘要】：本文對環(huán)境樣品中痕量雙酚A(BPA)的分離富集技術(shù)、磁性分子印跡技術(shù)、磁性表面分子印跡固相萃取技術(shù)、BPA分子印跡聚合物的制備技術(shù)的研究進(jìn)展和發(fā)展趨勢進(jìn)行了綜述;研究了 BPA的磁性表面分子印跡聚合物的合成方法和對環(huán)境水樣品中BPA的分離富集性能;合成了 BPA的磁性虛擬模板分子印跡聚合物,并將其作為磁性固相萃取的新型材料,應(yīng)用于塑料瓶裝飲品中痕量BPA的分離富集,建立了磁性虛擬模板分子印跡-固相萃取-高效液相色譜測定塑料瓶裝飲品中痕量BPA的新方法。將表面分子印跡技術(shù)與溶膠-凝膠方法相結(jié)合,在磁性核表面直接一步合成了均一、單分散、超順磁的雙酚A磁性分子印跡聚合物(MMIP),并通過磁性分析、傅里葉紅外光譜、X射線衍射分析、掃描電鏡、透射電鏡等方法對聚合物材料的形貌、結(jié)構(gòu)以及穩(wěn)定性進(jìn)行表征和分析,探究了 NH3·H2O的用量、溶劑組成、以及功能單體與交聯(lián)劑的比例對聚合物形貌的影響。在最佳條件下,對Fe3O4@MIP與Fe3O4@NIP在水溶液中的吸附性能進(jìn)行了研究。結(jié)果表明,此方法不僅簡單高效,避免了傳統(tǒng)過程中繁瑣的磁性核表面修飾過程,為聚合物材料的批量生產(chǎn)提供了一種新的方法,且合成的材料具有高吸附量(402.3μmolg-1)、快速的吸附速度(30 min)、良好的選擇性以及較高的循環(huán)適用性等優(yōu)點。以BPA的結(jié)構(gòu)類似物4,4'-二羥基聯(lián)苯(DDBP)作為虛擬模板分子,采用溶膠-凝膠法,在四氧化三鐵表面直接一步合成了 BPA的磁性虛擬模板分子印跡聚合物(BPA-DMMIP),對BPA-DMMIP進(jìn)行了紅外光譜、透射電鏡、掃描電鏡的表征,評價了虛擬模板表面印跡聚合物的吸附性能。結(jié)果表明:該虛擬模板聚合物對BPA有較大的吸附容量(444.6 μmol g-1),對BPA的吸附在30 min即可達(dá)到平衡,并顯示了對BPA的高選擇性和特別的親和力。此外,DMMIP避免了模板分子BPA的泄露,也極大簡化了固相萃取過程,為建立環(huán)境樣品中痕量BPA的分析測定方法奠定了基礎(chǔ)�；诖判苑肿佑≯E固相萃取的方法,將磁性虛擬模板分子印跡聚合物(DMMIP)材料應(yīng)用于塑料瓶裝飲品中BPA的分離富集。探究了吸附劑用量、溶液pH、洗脫液組成以及洗脫時間等因素對固相萃取回收率的影響,建立了DMMIP-SPE-HPLC測定痕量BPA的新方法。結(jié)果表明,在最佳條件下,BPA在30 s即可從DMMIP材料上洗脫下來,方法的富集倍數(shù)達(dá)400倍時回收率仍然大于899%,且對磁性固相萃取的吸附-洗脫過程重復(fù)6次后仍具有較好的回收率。此外,通過加標(biāo)回收法測定了塑料瓶裝飲品中的BPA,方法的回收率為88.6-99.5%,最低檢測限(LOD)為0.083 ngmL-1,相對標(biāo)準(zhǔn)偏差均低于9.5%。
[Abstract]:In this paper, the separation and enrichment of BPA in environmental samples, magnetic molecular imprinting, and molecular imprinted solid phase extraction (SPE) of magnetic surface are reviewed in this paper, and the research progress and development trend of BPA molecularly imprinted polymers are reviewed. The synthesis and separation and enrichment of BPA from environmental water samples of BPA were studied, and the magnetic virtual template molecularly imprinted polymer of BPA was synthesized and used as a new material for magnetic solid phase extraction (SPE). A new method for the determination of trace BPA in plastic bottled drinks by high performance liquid chromatography (HPLC) and imprinting of magnetic virtual template molecular imprinting solid phase extraction (SPE) has been developed for the separation and enrichment of trace BPA in plastic bottled drinks. A homogeneous, monodisperse, super-paramagnetic bisphenol A magnetic molecularly imprinted polymer was synthesized by combining the surface molecular imprinting technique with the sol-gel method. The morphology, structure and stability of the polymer were characterized and analyzed by Fourier transform infrared spectroscopy (FTIR), scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The amount of NH3 H2O and the composition of the solvent were investigated. And the influence of the ratio of functional monomer to crosslinking agent on the morphology of polymer. The adsorption properties of Fe3O4@MIP and Fe3O4@NIP in aqueous solution were studied under the optimum conditions. The results show that this method is not only simple and efficient, but also avoids the complicated surface modification process of magnetic nuclei in the traditional process, and provides a new method for batch production of polymer materials. The synthesized material has the advantages of high adsorption capacity of 402.3 渭 mol g-1g ~ (-1), fast adsorption rate of 30 min, good selectivity and high cycle applicability. The magnetic virtual template molecular imprinted polymer (BPA-DMMIP) of BPA was synthesized by sol-gel method using the structural analogue of BPA, 4H4 (4-dihydroxybiphenyl) DDBP, as a virtual template molecule. The imprinted polymer BPA-DMMIPe of BPA was synthesized directly on the surface of Fe _ 2O _ 4 by sol-gel method. The IR spectra of the imprinted polymer (BPA-DMMIP-) of BPA were studied. The adsorption properties of imprinted polymers on the surface of virtual templates were evaluated by transmission electron microscopy (TEM) and scanning electron microscopy (SEM). The results show that the virtual template polymer has a large adsorption capacity of 444.6 渭 mol g-1g ~ (-1) on BPA, and the adsorption of BPA can reach equilibrium at 30 min. It also shows high selectivity and special affinity to BPA. In addition, DMMIP avoids the leakage of template molecule BPA and greatly simplifies the solid-phase extraction process, which lays a foundation for the determination of trace BPA in environmental samples. Based on the method of magnetic molecularly imprinted solid phase extraction, the magnetic virtual template molecularly imprinted polymer (DMMIP) was applied to the separation and enrichment of BPA in plastic bottles. The effects of the amount of adsorbent, pH of solution, composition of eluent and elution time on the recovery rate of solid phase extraction (SPE) were investigated. A new method for the determination of trace BPA by DMMIP-SPE-HPLC was established. The results showed that under the optimum conditions, DMMIP could be eluted from the DMMIP material at 30 s. The recovery rate was still greater than 899 when the enrichment ratio of the method was 400 times, and the adsorption-elution process of magnetic solid phase extraction was repeated for 6 times and still had a good recovery. In addition, the recovery rate of BPA in plastic bottled drinks was 88.6-99.5, the lowest detection limit was 0.083 ngmL-1, and the relative standard deviation was lower than 9.5%.
【學(xué)位授予單位】：中國科學(xué)技術(shù)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：O631.3

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 刁春鵬;李聰;彭輝;蔡艷紅;裴曉洋;;基于磁性多壁碳納米管的渦旋輔助分散基質(zhì)固相萃取-高效液相色譜檢測水中雙酚A[J];中國環(huán)境監(jiān)測;2016年05期

2 韋壽蓮;劉玲;黎京華;汪洪武;劉永;;雙分子印跡聚合物微球選擇固相萃取環(huán)境和食品樣品中壬基酚和雙酚A[J];分析化學(xué);2015年01期

3 劉智敏;許志剛;何素瓊;毛翠萍;韓東方;王聯(lián)廣;;環(huán)境雌激素雙酚A的樣品前處理技術(shù)與分析檢測研究進(jìn)展[J];云南師范大學(xué)學(xué)報(自然科學(xué)版);2012年06期

4 焦艷娜;丁利;李暉;傅善良;王曉兵;王利兵;;加速溶劑萃取-GC-MS/MS法測定食品接觸材料中雙酚A、雙酚F及其衍生物的殘留量[J];包裝工程;2011年15期

5 徐靖;劉娟;金江嵐;;分子印跡基質(zhì)固相分散-超高效液相色譜法測定兒童玩具中雙酚A[J];理化檢驗(化學(xué)分冊);2011年06期

6 吳新華;丁利;肖家勇;龍妍嬌;許宙;李忠海;王利兵;;單分散磁性亞微米粒子固相萃取-液相色譜-串聯(lián)質(zhì)譜法測定牛奶中的雙酚A[J];色譜;2011年05期

7 李魚;劉建林;翦英紅;;分散液液微萃取-柱前衍生-高效液相色譜法測定水樣中雙酚A[J];分析化學(xué);2009年10期

8 宣棟j;陳靜;;固相萃取-高效液相色譜法測定嬰幼兒奶瓶中溶出的雙酚A[J];現(xiàn)代預(yù)防醫(yī)學(xué);2008年23期

9 張奎文;葉賽;那廣水;姚子偉;關(guān)道明;;高效液相色譜-串聯(lián)質(zhì)譜法測定環(huán)境水體中雙酚A、辛基酚、壬基酚[J];分析試驗室;2008年08期

10 楊本曉;唐瑾;鮮鳴;于紅霞;;雙酚A分子印跡聚合物的制備及其在環(huán)境監(jiān)測中的應(yīng)用初探[J];河南科學(xué);2007年06期

相關(guān)碩士學(xué)位論文 前1條

1 馬昊天;介孔硅基分子印跡聚合物的制備和吸附性能研究[D];哈爾濱工業(yè)大學(xué);2012年

，

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