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食品成分的高靈敏伏安檢測(cè)方法研究

發(fā)布時(shí)間:2018-03-12 09:06

  本文選題:食品分析 切入點(diǎn):石墨烯 出處:《鄭州大學(xué)》2017年碩士論文 論文類型:學(xué)位論文


【摘要】:石墨烯(Graphene)作為一種新型的碳納米材料有多種優(yōu)異性能,如良好的機(jī)械強(qiáng)度、大的比表面積以及好的導(dǎo)電性。石墨烯層與層之間存在π-π堆積和較強(qiáng)的范德華力,容易造成石墨烯的團(tuán)聚,很難均勻分散于水中,這些不利的因素嚴(yán)重影響其在電分析化學(xué)中的應(yīng)用。通過(guò)表面功能化的手段來(lái)解決這一問(wèn)題,使石墨烯的優(yōu)良性能得以充分的發(fā)揮。另外,功能化試劑有利于進(jìn)一步連接或負(fù)載金屬納米粒子,從而賦予石墨烯復(fù)合材料更為優(yōu)異的電化學(xué)性能。本文利用高分子聚合電解質(zhì)對(duì)石墨烯表面進(jìn)行功能化修飾,并進(jìn)一步在其表面負(fù)載金屬納米粒子。通過(guò)納米復(fù)合物的協(xié)同作用,構(gòu)筑了幾種性能優(yōu)異的電化學(xué)傳感器。探討了幾種食品成分在所構(gòu)筑傳感器上的電化學(xué)行為,為食品分析檢測(cè)提供了方法學(xué)的參考和依據(jù)。主要研究工作如下:(1)采用改進(jìn)的Hummer方法由天然石墨粉制得氧化石墨烯(GO),再以水合肼為還原劑進(jìn)行還原,同時(shí)加入聚苯乙烯磺酸鈉(PSS),制備成PSS功能化石墨烯(PSS-GR)復(fù)合材料。運(yùn)用簡(jiǎn)單的滴涂法構(gòu)筑了PSS-GR/GCE,并將其應(yīng)用于橙黃II的檢測(cè)。通過(guò)線性掃描伏安法(LSV)建立了對(duì)橙黃II的電化學(xué)檢測(cè)方法,線性范圍為3×10-8-5×10-6 mol L-1,檢測(cè)限為1×10-8 mol L-1,并將該傳感器成功地應(yīng)用于食品樣品中橙黃II的檢測(cè)。(2)通過(guò)綠色還原法制備了L-谷胱甘肽(GSH)功能化石墨烯(GR)。GSH分子中的巰基和氧化石墨烯(GO)上的環(huán)氧基通過(guò)親質(zhì)子的開(kāi)環(huán)反應(yīng)使得GSH以共價(jià)鍵結(jié)合在GO上,然后將GO還原,得到GSH修飾的石墨烯(GSH-GR)復(fù)合材料,將其滴涂在玻碳電極表面,制得GSH-GR/GCE伏安傳感器。該傳感器對(duì)蘆丁具有較強(qiáng)的富集能力和優(yōu)異的伏安響應(yīng)性能。在最佳檢測(cè)條件下利用方波伏安技術(shù)(SWV),得到對(duì)蘆丁響應(yīng)較寬的線性范圍(5×10-9-1×10-6 mol L-1),以及較低的檢測(cè)限(7×10-10 mol L-1)。此外,所制備的傳感器成功用于實(shí)際樣品中蘆丁的分析檢測(cè)。(3)利用非共價(jià)鍵合法合成聚二烯丙基二甲基氯化銨(PDDA)功能化石墨烯(GR)/鉑納米粒子(Pt NPs)復(fù)合材料。用紫外-可見(jiàn)光譜(UV-vis),傅立葉變換紅外光譜(FTIR),透射電鏡(TEM)和X-射線粉末衍射(XRD)對(duì)復(fù)合材料進(jìn)行了表征。將該復(fù)合材料用于對(duì)玻碳電極的修飾,得到的電化學(xué)伏安傳感器可實(shí)現(xiàn)對(duì)沒(méi)食子酸的靈敏檢測(cè)。在最優(yōu)條件下,通過(guò)方波伏安法(SWV)獲得較寬的線性范圍(3×10-8-1×10-6 mol L-1)和較低的檢測(cè)限(7×10-9 mol L-1)。所建立的伏安方法應(yīng)用于實(shí)際樣品中沒(méi)食子酸的檢測(cè)并得到滿意的結(jié)果。(4)通過(guò)超聲水浴方法合成鈀納米粒子摻雜聚苯乙烯磺酸鈉功能化石墨烯(PSS-GR-Pd)復(fù)合材料。用紫外-可見(jiàn)光譜(UV-vis),傅立葉變換紅外光譜(FTIR),透射電鏡(TEM)和X-射線衍射(XRD)對(duì)復(fù)成材料進(jìn)行表征。PSS-GR-Pd修飾玻碳電極對(duì)莧菜紅具有優(yōu)良的電化學(xué)響應(yīng),基于此建立了對(duì)莧菜紅的高靈敏伏安測(cè)定方法。在最優(yōu)實(shí)驗(yàn)條件下,通過(guò)差示脈沖伏安法(DPV),獲得了較寬的線性范圍(1×10-7-9×10-6 mol L-1)和較低的檢測(cè)限(7×10-9 mol L-1)。建立的檢測(cè)方法成功地應(yīng)用于飲料中莧菜紅的檢測(cè),結(jié)果滿意。
[Abstract]:Shi Moxi (Graphene) as a new type of carbon nano materials have many excellent properties, such as good mechanical strength, large specific surface area and good conductivity. There is a pi pi accumulation and strong van Edward forces between the graphene layers, easy to cause the graphene reunion, it is difficult to evenly disperse in the water, these factors seriously affect its application in Electroanalytical Chemistry. To solve this problem by means of surface functionalization, the excellent properties of graphene into full play. In addition, functional reagents is conducive to further connect or load metal nanoparticles, thus giving graphene composites more electrochemical properties excellent. The polymer electrolyte for functionalization of graphene surface, and further supported metal nanoparticles on its surface. The synergistic effect of nano composite, build a few Electrochemical sensor with excellent properties is discussed. Several kinds of food ingredients in the construction of electrochemical behavior on the sensor for food analysis provides reference and basis for the detection methodology. The main research work is as follows: (1) to graphene oxide by natural graphite powder using improved Hummer method (GO), and then restored using hydrazine as reducing agent and adding sodium polystyrene sulfonate (PSS), prepared PSS functionalized graphene (PSS-GR) composite material. The use of a simple drop coating method to build PSS-GR/GCE, and applied to detect orange II. By linear sweep voltammetry (LSV) was established for electrochemical detection method orange II, the linear range of 3 * 10-8-5 * 10-6 mol L-1, the detection limit is 1 * 10-8 mol L-1, and the detection of the sensor has been successfully applied in food samples of orange II. (2) L- was prepared through the green reduction of glutathione (GSH) function Graphene (GR) and thiol graphene oxide in the molecule of.GSH (GO) on the GSH epoxy covalently bound to GO by ring opening reaction of proton affinity, and the reduction of GO, GSH modified graphene (GSH-GR) composite material is coated on the surface of glassy carbon electrode. Preparation of GSH-GR/GCE electrochemical sensor. The sensor has strong enrichment capacity and excellent performance. The voltammetric response of rutin by square wave voltammetry in the optimal detection conditions (SWV), get a wide range of linear response of rutin (5 * 10-9-1 * 10-6 mol L-1), and low detection limit (7 x 10-10 mol L-1). In addition, the prepared sensor successfully used to detect Rutin in real samples. (3) the use of non covalent binding synthesis of poly diallyl dimethyl ammonium chloride (two PDDA) functionalized graphene (GR) / Pt nanoparticles (Pt NPs) composite material. By UV Vis spectroscopy (UV-v is),鍌呯珛鍙跺彉鎹㈢孩澶栧厜璋,

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