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1、西南科技大学硕士研究生学位论文 第 I 页Preparation of Methoxy Polyethylene Glycol Stabilized Gold Nanoparticles and Their Applications for Detection and Absorption of Acrylamide摘 要本文以聚乙二醇单甲醚(PEG)为原料，制备了聚乙二醇单甲醚纳米金（PEG-纳米金） ，并将聚乙二醇巯基功能化后制备了巯基化聚乙二醇单甲醚纳米金（PEG-HS-纳米金） ，然后将两种纳米金分别用于有毒小分子丙烯酰胺的检测和吸附上。建立了一种基于聚乙二醇单甲醚稳定的纳米金可视化检
2、测丙烯酰胺(AA)的新方法，并用透射电子显微镜（TEM） 、紫外可见光光度计(UV)、激光粒度分析仪(DLS)对聚乙二醇纳米金进行测试分析。结果表明：该聚乙二醇纳米金核呈分散均匀的规则球体，且其平均粒径为 19nm。颗粒整体（纳米金核和表面稳定剂）粒径集中分布在 40 nm。浓度为 0.004 mg/mL 的丙烯酰胺能使聚乙二醇纳米金发生团聚，胶体由红色变成紫色，浓度在 0.004 mg/mL-0.032 mg/mL 之间时，团聚程度随浓度的增加而增加，同时颗粒整体粒径依次增大到 170 nm、250 nm、600 nm。相同条件下，N, N-二甲基丙烯酰胺(DMAA)不能使聚乙二醇纳米金发生
3、团聚。因此，可用该方法简单、快速的实现丙烯酰胺选择性检测。将巯基化聚乙二醇纳米金用于丙烯酰胺吸附，研究了其吸附性能、吸附机理以及循环利用。氢核磁（1H-NMR） 、高效液相色谱（HPLC） 、紫外可见分光光谱（UV） 、透射电子显微电镜（TEM） 、激光粒度分析仪（DLS）等测试表明：该巯基化聚乙二醇纳米金在有机溶剂和水溶液中均能吸附丙烯酰胺，但不吸附 N, N-二甲基丙烯酰胺，这种吸附来源于丙烯酰胺的氢原子与巯基化聚乙二醇的氧原子之间的氢键。二氯甲烷中每个巯基化聚乙二醇纳米金平均吸附 25772 个丙烯酰胺分子，水溶液中每个巯基化聚乙二醇纳米金平均吸附 22420 个丙烯酰胺分子，西南科技大
4、学硕士研究生学位论文 第 II 页比二氯甲烷中少，这可能是水溶液中水分子使丙烯酰胺与聚乙二醇之间的氢键作用减弱。另外，该巯基化聚乙二醇纳米金前 4 次循环团聚较少，循环 5 次之后，团聚量超过 50%，这可能是多次离心使纳米金产出团聚引起的。因此，该巯基化聚乙二醇纳米金可能成为新型可循环利用的有毒小分子吸附剂。关键词：聚乙二醇；纳米金；丙烯酰胺；检测；吸附AbstractIn this paper, methoxy polyethylene glycol(PEG) stabilized gold nanoparticles（PEG-AuNPs）and thiol functionalized
5、PEG stabilized gold nanoparticles (PEG-HS-AuNPs) have been prepared. Then these two gold nanoparticles were used in the detection and adsorption of the toxic small molecules, e.g. acrylamide, respectively.Firstly, the novel visual method for the detection of acrylamide by PEG-AuNPs has been develope
6、d. The PEG-AuNPs were characterized by transmission electron microscopy (TEM), ultraviolet spectrophotometer (UV), Dynamic Light Scattering (DLS). The results indicated that the size of the spherical AuNP core was 19 nm and well dispersed. In addition, the size of PEG-AuNPs (including Au cores and s
7、urface stabilizers) was around 40 nm. Significantly, 0.004 mg/mL acrylamide could induce the aggregation of the PEG-AuNPs, which caused the color changing of the colloidal solution from red to purple. The aggregations of AuNPs enhanced with the increase of acrylamide concentration from 0.004 mg/mL t
8、o 0.032 mg/mL. However, N, N-dimethylacrylamide could not induce aggregation of PEG-AuNPs under the same condition. Therefore, this method could provide new opportunities for the rapid, simple and selective detection of acrylamide.Secondly, PEG-HS-AuNPs were used to adsorb acrylamide. The adsorption
9、 capacity, adsorption mechanism and recycling have been studied. The PEG-HS-AuNPs were characterized by 1H-NMR, HPLC, TEM, UV and DLS, and the results indicated that the PEG-HS-AuNPs could adsorb acrylamide both in hydrophobic and aqueous media, but could not adsorb N, N-dimethylacrylamide. The adso
10、rption was attributed to the hydrogen bonding between the proton in acrylamide and the oxygen atom in the PEG-HS-AuNPs. Each PEG-HS-AuNP could adsorb about 25772 acrylamide molecules 西南科技大学硕士研究生学位论文 第 III 页in CH2Cl2, and about 22420 acrylamide molecules in aqueous media, which was less than that in
11、CH2Cl2, This may due to the presence of the H2O in the aqueous media which weakened the hydrogen bonding between the PEG-HS-AuNPs and the acrylamide. In addition, the PEG-HS-AuNPs could recycled 4 times with small agglomeration, and after 5 times, more than 50% gold nanoparticles are aggregated. Thi
12、s may due to the agglomeration during centrifugation process. Therefore, PEG-HS-AuNPs could be a new recyclable adsorbent for toxic small molecules.Keywords: methoxy polyethylene glycol; gold nanoparticles; acrylamide; detection; adsorption西南科技大学硕士研究生学位论文 第 I 页目目 录录1 绪论 .11.1 聚乙二醇性质及其应用 .11.1.1 聚乙二醇
13、性质简介 .11.1.2 聚乙二醇及其衍生物的应用 .21.2 纳米金制备方法及其应用 .51.2.1 纳米金的制备方法 .51.2.2 功能化巯基配体修饰纳米金的方法 .81.2.3 纳米金的应用 .91.3 聚乙二醇纳米金的应用 .121.4 丙烯酰胺的检测及吸附方法 .131.4.1 丙烯酰胺的检测方法 .131.4.2 丙烯酰胺吸附方法 .161.5 本课题研究意义和主要研究内容.171.5.1 本课题研究意义 .171.5.2 本课题主要研究内容 .182 聚乙二醇纳米金的制备及表征 .192.1 引言 .192.2 实验部分 .192.2.1 主要药品及仪器 .192.2.2 PEG-纳米金的制备 .202.2.3 PEG-HS-纳米金的制备 .212.2.4 样品表征方法和仪器 .242.3 结果与讨论 .252.3.1 UV 光谱分析 PEG-纳米金 .252.3.2 TEM 分析 PEG-纳米金 .
