2-甲氧基雌二醇限進(jìn)介質(zhì)分子印跡聚合物的制備及應(yīng)用
發(fā)布時(shí)間:2019-01-11 19:18
【摘要】:限進(jìn)介質(zhì)分子印跡聚合物具有較高的選擇性、親水性、穩(wěn)定性等優(yōu)點(diǎn),已成為分析工作者關(guān)注的熱點(diǎn),在藥物傳遞系統(tǒng)、食品、藥品及環(huán)境監(jiān)測(cè)等領(lǐng)域中具有良好的應(yīng)用前景。本研究采用沉淀聚合法制備了2-甲氧基雌二醇(2-ME)限進(jìn)介質(zhì)分子印跡聚合物,該聚合物對(duì)2-ME具有良好的特異性識(shí)別同時(shí)可避免蛋白的不可逆吸附。將其作為固相萃取填料,在復(fù)雜生物樣品中2-ME的專屬分析和檢測(cè)中可發(fā)揮重要作用。主要研究?jī)?nèi)容摘要如下: 1.2-ME限進(jìn)介質(zhì)分子印跡聚合物的制備及評(píng)價(jià) 本研究采用17β-雌二醇為偽模板分子,以沉淀聚合法制備2-ME限進(jìn)介質(zhì)分子印跡聚合物避免了模板滲漏對(duì)痕量分析的影響,并對(duì)制備條件進(jìn)行了優(yōu)化。以傅立葉紅外光譜、掃描電子顯微鏡、熱重分析儀及激光納米粒度儀對(duì)聚合物進(jìn)行表征。實(shí)驗(yàn)考察了聚合物對(duì)2-ME的吸附選擇性及蛋白吸附能力,并以等溫吸附法測(cè)定聚合物吸附特性,以Scatchard模型對(duì)等溫吸附曲線進(jìn)行擬合。本研究制備的聚合物呈微球狀結(jié)構(gòu)、具有良好的親水性,能明顯減少蛋白的不可逆吸附,并對(duì)2-ME具有特異性識(shí)別能力。 2.限進(jìn)介質(zhì)分子印跡聚合物固相萃取-高效液相色譜聯(lián)用分析血漿中2-ME 本研究以限進(jìn)介質(zhì)分子印跡聚合物為固相萃取填料,通過(guò)固相萃取-高效液相色譜聯(lián)用技術(shù),建立了特異性強(qiáng)、回收率高的血漿樣品2-ME分析新方法。方法檢測(cè)限為0.02μg/ml,,線性范圍為0.06-20μg/ml,日內(nèi)精密度為2.9%-9.3%,日間精密度為3.5%-11.9%,回收率為99.10%-101.00%。該方法應(yīng)用于2-甲氧基雌二醇血漿樣品的分析,所得結(jié)果較滿意。為建立快速、有效、專屬的復(fù)雜生物樣品檢測(cè)方法奠定了基礎(chǔ)。 3.限進(jìn)介質(zhì)分子印跡聚合物整體柱的制備及應(yīng)用 本研究采用原位聚合法制備了限進(jìn)介質(zhì)分子印跡整體柱?疾炝苏w柱蛋白吸附性及選擇性。將制備的整體柱應(yīng)用于血漿中2-ME的在線萃取、富集。結(jié)果表明,該整體柱能在線去除生物樣品中大分子蛋白及干擾物質(zhì),同時(shí)對(duì)分析藥物具有較好的保留,可實(shí)現(xiàn)血樣中2-ME快速、便捷、有效的富集分析。
[Abstract]:Molecularly imprinted polymers (MIPs) with limited media have become the focus of attention due to their high selectivity, hydrophilicity and stability, and have a good application prospect in the fields of drug delivery system, food, medicine and environmental monitoring. In this study, 2-methoxyestradiol (2-ME) molecularly imprinted polymer was prepared by precipitation polymerization. The polymer has good specificity for 2-ME recognition and can avoid irreversible adsorption of protein. It can play an important role in the analysis and detection of 2-ME in complex biological samples. The main contents of this study are summarized as follows: preparation and evaluation of imprinted polymer with 1.2-ME as limiting medium in this study, 17 尾 -estradiol was used as pseudo-template molecule, and 17 尾 -estradiol was used as pseudo-template molecule. Molecular imprinted polymers with 2-ME limiting medium were prepared by precipitation polymerization to avoid the influence of template leakage on trace analysis and the preparation conditions were optimized. The polymer was characterized by Fourier transform infrared spectroscopy, scanning electron microscope, thermogravimetric analyzer and laser nanocrystalline analyzer. The adsorption selectivity and protein adsorption ability of polymer to 2-ME were investigated. The adsorption characteristics of polymer were measured by isothermal adsorption method. The isothermal adsorption curve was fitted by Scatchard model. The polymer prepared in this study has a microsphere structure, good hydrophilicity, can significantly reduce the irreversible adsorption of protein, and has a specific recognition ability to 2-ME. 2. Determination of 2-ME in Plasma by Solid-Phase extraction and High performance liquid Chromatography with Molecular imprinting Polymer as Solid-Phase extraction packing, the study was carried out by using solid-phase extraction-high performance liquid chromatography (HPLC), using molecularly imprinted polymer as solid phase extraction filler. A new method for 2-ME analysis of plasma samples with strong specificity and high recovery was established. The detection limit was 0.02 渭 g / ml, the linear range was 0.06-20 渭 g / ml, the intra-day precision was 2.9-9.3, and the daytime precision was 3.5-11.9.The recovery was 99.10-101.00. The method has been applied to the analysis of 2-methoxyestradiol plasma samples with satisfactory results. It lays a foundation for the establishment of a rapid, effective and exclusive method for the detection of complex biological samples. 3. Preparation and Application of molecularly imprinted Polymer monolithic column with confined medium in this study the molecular imprinted monolithic column was prepared by in-situ polymerization. The adsorption and selectivity of monolithic column protein were investigated. The prepared monolithic column was applied to the on-line extraction and enrichment of 2-ME in plasma. The results showed that the monolithic column could remove macromolecular proteins and interfering substances from biological samples on line, and had a good retention for the analysis of drugs, and could achieve rapid, convenient and effective enrichment and analysis of 2-ME in blood samples.
【學(xué)位授予單位】:鄭州大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2014
【分類號(hào)】:R943
[Abstract]:Molecularly imprinted polymers (MIPs) with limited media have become the focus of attention due to their high selectivity, hydrophilicity and stability, and have a good application prospect in the fields of drug delivery system, food, medicine and environmental monitoring. In this study, 2-methoxyestradiol (2-ME) molecularly imprinted polymer was prepared by precipitation polymerization. The polymer has good specificity for 2-ME recognition and can avoid irreversible adsorption of protein. It can play an important role in the analysis and detection of 2-ME in complex biological samples. The main contents of this study are summarized as follows: preparation and evaluation of imprinted polymer with 1.2-ME as limiting medium in this study, 17 尾 -estradiol was used as pseudo-template molecule, and 17 尾 -estradiol was used as pseudo-template molecule. Molecular imprinted polymers with 2-ME limiting medium were prepared by precipitation polymerization to avoid the influence of template leakage on trace analysis and the preparation conditions were optimized. The polymer was characterized by Fourier transform infrared spectroscopy, scanning electron microscope, thermogravimetric analyzer and laser nanocrystalline analyzer. The adsorption selectivity and protein adsorption ability of polymer to 2-ME were investigated. The adsorption characteristics of polymer were measured by isothermal adsorption method. The isothermal adsorption curve was fitted by Scatchard model. The polymer prepared in this study has a microsphere structure, good hydrophilicity, can significantly reduce the irreversible adsorption of protein, and has a specific recognition ability to 2-ME. 2. Determination of 2-ME in Plasma by Solid-Phase extraction and High performance liquid Chromatography with Molecular imprinting Polymer as Solid-Phase extraction packing, the study was carried out by using solid-phase extraction-high performance liquid chromatography (HPLC), using molecularly imprinted polymer as solid phase extraction filler. A new method for 2-ME analysis of plasma samples with strong specificity and high recovery was established. The detection limit was 0.02 渭 g / ml, the linear range was 0.06-20 渭 g / ml, the intra-day precision was 2.9-9.3, and the daytime precision was 3.5-11.9.The recovery was 99.10-101.00. The method has been applied to the analysis of 2-methoxyestradiol plasma samples with satisfactory results. It lays a foundation for the establishment of a rapid, effective and exclusive method for the detection of complex biological samples. 3. Preparation and Application of molecularly imprinted Polymer monolithic column with confined medium in this study the molecular imprinted monolithic column was prepared by in-situ polymerization. The adsorption and selectivity of monolithic column protein were investigated. The prepared monolithic column was applied to the on-line extraction and enrichment of 2-ME in plasma. The results showed that the monolithic column could remove macromolecular proteins and interfering substances from biological samples on line, and had a good retention for the analysis of drugs, and could achieve rapid, convenient and effective enrichment and analysis of 2-ME in blood samples.
【學(xué)位授予單位】:鄭州大學(xué)
【學(xué)位級(jí)別】:碩士
【學(xué)位授予年份】:2014
【分類號(hào)】:R943
【共引文獻(xiàn)】
相關(guān)期刊論文 前6條
1 陳燁;許秀艷;王超;滕恩江;呂怡兵;;地表水中有機(jī)磷農(nóng)殘測(cè)定的前處理方法比較[J];中國(guó)測(cè)試;2014年01期
2 劉慧慧;宮向紅;徐英江;鄒榮婕;李佳蔚;鄧旭修;張秀珍;;固相萃取-高效液相色譜法同時(shí)測(cè)定海米中10種合成色素[J];食品科學(xué);2014年04期
3 吳宗遠(yuǎn);李小燕;蘇曉o
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