本文關(guān)鍵詞： 分子印跡聚合物 樣品前處理 整體材料 固相微萃取　出處：《昆明理工大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：分子印跡微萃取技術(shù)結(jié)合了分子印跡技術(shù)和微萃取技術(shù)兩者的優(yōu)點(diǎn),并應(yīng)用于樣品前處理過程中。由于分子印跡聚合物具有選擇性高、抗干擾能力強(qiáng)、樣品用量小、有機(jī)溶劑用量少,可用于復(fù)雜樣品中痕量目標(biāo)分析物的分離與富集。本論文介紹了分子印跡微萃取材料的特點(diǎn),并綜述了其原理、制備方法、表征手段以及材料形式。同時(shí)開展了以雌二醇、雙酚F和硝基苯酚為模板的分子印跡聚合物的應(yīng)用研究,主要內(nèi)容如下:1.雌二醇分子印跡整體材料的制備與應(yīng)用研究:以雌二醇為模板分子,采用原位聚合法合成分子印跡整體材料;研究了雌二醇分子印跡整體材料的表面形貌和萃取性能,優(yōu)化了萃取條件;建立了雌二醇MIP整體材料聯(lián)用HPLC的分析方法,線性范圍為0.5-50μg/L,檢出限為0.1 μg/L(S/N=3);將雌二醇分子印跡整體材料聯(lián)用高效液相色譜應(yīng)用于實(shí)際水樣中三種雌激素的萃取分析,加標(biāo)濃度為20 μg/L時(shí),兩種水樣加標(biāo)的回收率在68.22%-102.52%,以及67.65%-103.72%,RSDs 在 3.18%-6.43%和 2.43%-5.70%之間(n=5)。2.雙酚F替代模板分子印跡整體材料的制備和應(yīng)用研究:以雙酚F為替代模板分子制備得到分子印跡聚合物材料;研究了 BPF分子印跡整體材料的表面形貌、萃取性能,優(yōu)化了 MIP整體材料的萃取條件,建立了 BPF-MIP整體材料聯(lián)用HPLC的分析方法,并用于實(shí)際水樣中BPA的萃取分析,線性范圍為0.01-15μg/L(r=0.9998),檢出限為0.003 μg/L(S/N=3);兩種水樣的回收率分別為65.56%-88.84%和70.48%-87.06,RSDs分別 2.15%-8.93%和1.30%-8.21%。3.對硝基苯酚環(huán)糊精分子印跡吸附萃取涂層的制備及其應(yīng)用研究:對硝基苯酚為模板分子,采用四種新型環(huán)糊精衍生物為功能單體,通過原位聚合法合成分子印跡整體材料;研究了對硝基苯酚分子印跡吸附萃取涂層的表面形貌、萃取性能及協(xié)同作用,優(yōu)化了 MIP吸附萃取涂層的萃取條件,建立了 MIP吸附萃取涂層聯(lián)用HPLC的分析方法,線性范圍均為10-200 μg/L,硝基苯酚的檢出限為3μg/L,雙酚A檢出限為1.5μg/L;應(yīng)用于河水中三種硝基苯酚和BPA的萃取分析,其中對硝基苯酚、鄰硝基苯酚、間硝基苯酚和雙酚A的回收率在88.17%-104.54%之間,RSDs為0.54%-8.28%。
[Abstract]:The molecularly imprinted microextraction technology combines the advantages of both the molecular imprinting technique and the microextraction technology, and is applied in the sample pretreatment process. Because of the high selectivity, strong anti-interference ability and small sample dosage of the molecularly imprinted polymer, In this paper, the characteristics of molecularly imprinted microextraction materials are introduced, and their principles and preparation methods are summarized. At the same time, the application of imprinted polymers with estradiol, bisphenol F and nitrophenol as templates was studied. The main contents are as follows: 1. Preparation and application of estradiol molecularly imprinted monolayer: using estradiol as template molecule, in situ polymerization method was used to synthesize molecularly imprinted monolithic material; The surface morphology and extraction performance of estradiol molecularly imprinted monolithic materials were studied and the extraction conditions were optimized. A method for the analysis of estradiol MIP monolithic materials with HPLC was established. The linear range is 0.5-50 渭 g 路L ~ (-1) and the detection limit is 0.1 渭 g 路L ~ (-1) N ~ (-1) N ~ (3 +). When the standard concentration is 20 渭 g / L, the Estradiol molecularly imprinted whole material is used in the extraction analysis of three kinds of estrogens in the real water samples by high performance liquid chromatography. The recoveries of two kinds of water samples were between 68.22 and 102.52, and the RSDs were between 3.18-6.43% and 2.43-5.70%. The preparation and application of bisphenol F substitute template molecular imprinting materials were studied: using bisphenol F as substitute template molecule to obtain molecularly imprinted polymer materials; The surface morphology and extraction properties of BPF molecularly imprinted monolithic materials were studied. The extraction conditions of MIP monolithic materials were optimized. The analytical method of BPF-MIP monolithic materials combined with HPLC was established and applied to the extraction analysis of BPA in real water samples. The linear range was 0.01-15 渭 g / L ~ 0.9998 渭 g 路L ~ (-1) 路L ~ (-1) L ~ (-1), the detection limit was 0.003 渭 g / L ~ (-1) 渭 g 路L ~ (-1) N ~ (-1) N, the recoveries of the two water samples were 65.56% -88.84% and 70.48% -87.06% RSDs, respectively, 2.15-8.93% and 1.30-8.21 路3.The preparation and application of p-nitrophenol cyclodextrin molecular imprinting extraction coating were studied. Four new cyclodextrin derivatives were used as functional monomers to synthesize molecularly imprinted monolithic materials by in situ polymerization. The extraction conditions of MIP adsorption and extraction coating were optimized, and the analytical method of MIP adsorption and extraction coating combined with HPLC was established. The linear range is 10-200 渭 g / L, the detection limit of nitrophenol is 3 渭 g / L, and the detection limit of bisphenol A is 1.5 渭 g / L. The recoveries of m-nitrophenol and bisphenol A ranged from 88.17% to 104.54% and the RSDs were 0.54 -8.28%.
【學(xué)位授予單位】：昆明理工大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：X502;O631.3

【參考文獻(xiàn)】

相關(guān)期刊論文 前10條

1 劉帥;胡磊;楊明;;G蛋白偶聯(lián)雌激素受體1介導(dǎo)的環(huán)境雌激素效應(yīng)研究進(jìn)展[J];生態(tài)毒理學(xué)報(bào);2016年01期

2 楊靜;俞捷;楊孟雪;許潔;;環(huán)境雌激素暴露與糖尿病發(fā)病關(guān)系研究進(jìn)展[J];中國公共衛(wèi)生;2016年07期

3 劉蓉;鐘桐生;劉石泉;趙運(yùn)林;關(guān)懷昱;朱家會;;電聚合分子印跡傳感器測定黑茶中蘆丁的含量[J];化學(xué)研究與應(yīng)用;2015年08期

4 許志剛;馮鋒;劉智敏;楊保民;字富庭;何素瓊;;分子印跡聚合物微萃取樣品前處理技術(shù)研究（英文）[J];昆明理工大學(xué)學(xué)報(bào)(自然科學(xué)版);2014年04期

5 岳宗豪;趙歡;周一兵;;酚類環(huán)境雌激素對水生生物毒性效應(yīng)的研究進(jìn)展[J];生態(tài)毒理學(xué)報(bào);2014年02期

6 趙娜;胡小玲;管萍;宋任遠(yuǎn);田甜;張向榮;;乳液聚合法制備紅霉素分子印跡聚合物微球及其吸附性能[J];物理化學(xué)學(xué)報(bào);2014年01期

7 許志剛;湯令;陸遙;劉智敏;;兩種水溶性β-環(huán)糊精新型功能單體的合成研究[J];化學(xué)研究與應(yīng)用;2013年11期

8 李娟;王薈;;水中多種酚類化合物同步提取方法研究[J];中國環(huán)境監(jiān)測;2013年04期

9 許志剛;劉智敏;石杰蘭;陸遙;;環(huán)糊精分子印跡技術(shù)及其應(yīng)用研究[J];化學(xué)試劑;2013年01期

10 陸寬;朱秋勁;;基于β-環(huán)糊精的分子印跡技術(shù)識別機(jī)理及評價(jià)手段[J];功能材料;2012年S1期

，

本文編號：1504422