Preparation of Functionalized Fe3O4@SiO2 Magnetic Nanoparticles for Monoclonal Antibody Purification

Magnetic Fe₃O₄@SiO₂ nanoparticles with superparamagnetic properties were prepared via a reverse mi-croemulsion method at room temperature. The as-prepared samples were characterized by transmission electron mi-croscopy(TEM), X-ray diffractometry(XRD), and vibrating sample magnetometry(VSM). The Fe₃O₄@SiO₂ nanoparticles were modified by (3-aminopropyl)triethoxysilane(APTES) and subsequently activated by glutaraldehyde(Glu). Protein A was successfully immobilized covalently onto the Glu activated Fe₃O₄@SiO₂ nanoparticles. The adsorption capacity of the nanoparticles was determined on an ultraviolet spectrophotometer(UV) and approximately up to 203 mg/g of protein A could be uniformly immobilized onto the modified Fe₃O₄@SiO₂ magnetic beads. The core-shell of the Fe₃O₄@SiO₂ magnetic beads decorated with protein A showed a good binding capacity for the chime-ric anti-EGFR monoclonal antibody(anti-EGFR mAb). The purity of the anti-EGFR mAb was analyzed by virtue of HPLC. The protein A immobilized affinity beads provided a purity of about 95.4%.     

High-efficient Isolation of Plant Viral RNA via TMAOH-modified Fe3O4 Magnetic Nanoparticles

Magnetic nanoparticles show great potential in RNA enrichment and separation for rapid detection of viral infection.Fundamental studies on the interaction between RNA and nanoparticles with uniform size and surface property are necessary for designing better adsorbent and optimizing the conditions.In this study,monodispersed superparamagnetic magnetite（Fe3O4） nanoparticles were synthesized by thermal decomposition and modified with tetramethylammonium hydroxide[N（CH3）4OH,TMAOH] that become highly dispersible and stable in water.High-efficiency plant viral RNA adsorption onto TMAOH/Fe3O4 nanoparticles in the extracted solution of plant leaves was demonstrated.The changes of surface charge of TMAOH on the Fe3O4 nanoparticles with pH contribute to the RNA adsorption and elution.Separating viral RNA with magnetic nanoparticles could be a simple,quick andhighly efficient method.     

柠檬酸根辅助多元醇法制备直径和磁性可控的Fe_3O_4亚微球

以柠檬酸三钠作辅助剂,用多元醇溶剂热还原法制备了纳米晶粒和微球直径可控的、单分散的超顺磁Fe3O4亚微球.发现与铁原子有强亲和力的柠檬酸根能有效吸附在还原产生的初始Fe3O4纳米粒子表面,阻碍其晶粒生长和影响其静电排斥力的大小,从而能在较大范围内调控最终产物Fe3O4亚微球的直径和饱和磁化强度.改变柠檬酸根或铁盐浓度不但可以调控初始Fe3O4纳米粒子的粒径,而且可以在220-550nm范围内调控单分散Fe3O4亚微球的直径,从而得到粒径均一的超顺磁Fe3O4亚微球.     

Fast synthesis of dopamine-coated Fe3O4 nanoparticles through ligand-exchange method

A fast approach was described for the synthesis of water-dispersible monodisperse dopamine-coated Fe₃O₄ nanoparticles（DA-Fe₃O₄） with uniform size and shape via ligand-exchange of oleic acid on Fe₃O₄ using only 2 min.The prepared DA-Fe₃O₄ nanoparticles were characterized by transmission electron microscopy,Fourier transform infrared spectrometry,and vibrating sample magnetometer.The results indicated that the resulting DA-Fe₃O₄ nanoparticles had an average diameter of about 19.2 nm. The magnetic saturation value of the prepared DA-Fe₃O₄ nanoparticles was determined to be 72.87 emu/g,which indicating a well-established superparamagnetic property.     

Fe3O4纳米粒子修饰多壁碳纳米管的制备及在水和蜂蜜样品中痕量菊酯类农药分析中的应用

通过化学共沉淀法使Fe₃O₄纳米粒子负载于酸化多壁碳纳米管(AMWNTs)表面,得到Fe₃O₄/AMWNTs磁性纳米材料。该材料具有很好的磁响应度和分散性,将其用于富集痕量拟除虫菊酯类农药残留,结果证明该复合材料对菊酯类农药的吸附性能良好。通过对影响萃取性能的几种因素如离子强度、萃取时间和解吸时间依次进行优化,在最优条件下,建立了Fe₃O₄/AMWNTs磁性分散固相萃取-气相色谱测定6种菊酯类农药残留的分析方法。线性范围在0.5~50 μg/L之间,相关系数(R²)大于0.990,检出限为0.07~0.20 μg/L,精密度为3.8%~8.1%。该方法用于河水、鱼塘水和两种市售蜂蜜中菊酯类农药的残留分析,回收率高于78.4%。该方法操作简便、灵敏度高,能够满足环境水样及蜂蜜样品中痕量菊酯农药残留的分析需求。     

Combined investigation of experimental characterization and theoretic calculation on the structure of dextran-Fe3O4 clusters

Dextran-Fe₃O₄ hybrid clusters were fabricated by coprecipitating ferric and ferrous ions in the presence of dextran, and after characterization of these clusters combined with calculation based on classical nucleation theory, a structure model of these hybrid clusters was proposed. The hybrid cluster was believed including small Fe₃O₄ nanoparticles and dextran which acted as both nucleating agent and stabilizer, so that exist in both the inside of magnetite nanoparticles and the periphery of the hybrid clusters. Besides, the effects of W_CD (weight_{iron cation}:weight_dextran) and molecular weight of dextran on the size, morphology and magnetic property of clusters were also investigated in this paper. It was found that the variation of W_CD and molecular weight of dextran have great effect on the size of the hybrid clusters, but have almost no effect on the size of the Fe₃O₄ nanoparticles. The characterization of magnetic property demonstrated that the Fe₃O₄ nanoparticles are of a single domain and the saturation magnetization was affected by the size of dextran-Fe₃O₄ hybrid clusters.     

Aluminum-type superparamagnetic adsorbents: Synthesis and application on fluoride removal

Two effective types of superparamagnetic nano-scale adsorbents of bayerite/SiO₂/Fe₃O₄ have been synthesized via three sequential steps: chemical precipitation of Fe₃O₄, coating of SiO₂ on Fe₃O₄ using acidifying method, and further coating of bayerite (Al(OH)₃) on SiO₂/Fe₃O₄ adopting sol–gel (MASG) or homogeneous precipitation (MAHP) methods. The characteristics of MASG and MAHP were identified using the transmission electron microscopy (TEM) micrograph, scanning electron microscopy with energy dispersive X-ray spectroscopy (SEM/EDX), X-ray powder diffractometer (XRD), and superconducing quantum interference device (SQUID). Removal of fluoride from aqueous solution was examined to evaluate the adsorptive capacity of MASG, MAHP, and commercial activated alumina (CA), and the effects of enclosure of Fe₃O₄ with SiO₂ for SiO₂/Fe₃O₄, MASG, and MAHP particles. Among the adsorbents tested under the same experimental condition, MASG is the most effective adsorbent, of which the adsorption capacities are 38 g/kg (based on adsorbent mass of adsorption in terms of equilibrium constant q_L of Langmuir isotherm), and can compete with CA even at a high pH value. The innovative superparamagnetic adsorbents synthesized in this study possess physicochemical stability at pH range of 6–8 and great potential in the adsorption processes due to not only their high adsorption capacity but also the conveniently magnetic separation which can overcome the difficulty in solid–liquid separation for nano-particles in solutions.     

磁性介孔纳米粒子的制备及对抗癌药紫杉醇的传输

以十六烷基溴化铵(CTAB)为结构导向剂, 正硅酸乙酯(TEOS)为硅源, 在碱性环境下经过自组装过程对单分散性磁性Fe₃O₄纳米粒子进行包覆, 制备出磁性硅基介孔纳米粒子Fe₃O₄@SiO₂. 结合X射线衍射、 傅里叶变换红外光谱(FTIR)、 透射电子显微镜(TEM)以及氮气吸附-脱附等技术对Fe₃O₄@SiO₂粒子进行表征. 结果表明Fe₃O₄@SiO₂纳米粒子具有球形形貌, 平均直径约为150 nm, 蠕虫状介孔结构, 比表面积为932 m²/g, 孔径为2.5 nm且分布较均匀, 包覆后Fe₃O₄的结构得以保持, 同时材料具有很好的磁响应能力. 以抗癌药紫杉醇(Paelitaxel, TXL)为模型药物进行负载, 实验结果表明, Fe₃O₄@SiO₂对TXL的负载能力为80 mg/g, TXL-Fe₃O₄@SiO₂对TXL的缓释时间持续120 h以上, 累积释放量达到30 mg/g. 通过噻唑蓝比色(MTT)法测量了TXL-Fe₃O₄@SiO₂粒子对体外培养的HeLa细胞的细胞毒性, 与相同浓度的TXL相比, TXL-Fe₃O₄@SiO₂对HeLa细胞的抑制率明显增高.     

Fe3O4@Au核-壳纳米复合材料的制备及对农药福美双的SERS检测研究

首先采用热分解法制备了Fe₃O₄纳米材料, 再将其作为磁性核, 分别采用种子沉积法和种子介导生长法制备了Fe₃O₄-Au核-卫星纳米复合材料和Fe₃O₄@Au核-壳纳米复合材料, 并对其形貌和性能进行了表征分析. 结果表明, 所制备的Fe₃O₄-Au核-卫星和Fe₃O₄@Au核-壳纳米复合材料粒径均匀, Au纳米颗粒均匀沉积/包覆在Fe₃O₄纳米材料表面, 且样品均具有良好的磁响应性. 使用4-氨基苯硫酚(4-ATP)作为拉曼探针分子, 对比了这两种纳米复合材料作为SERS基底时的拉曼信号增强效果. 结果显示, Fe₃O₄@Au核-壳纳米复合材料是更优秀的SERS基底, 且该SERS基底具有良好的信号再现性. 最后, 使用Fe₃O₄@Au核-壳纳米复合材料作为SERS基底, 成功地在苹果皮上检测出残留福美双的SERS信号.     

Pd/Fe3O4-C催化剂对甲醇、乙醇和丙醇氧化的电催化活性

制备对醇氧化反应具有优异电活性的钯催化剂是醇燃料电池研究的重要内容。本文用硼氢化钠还原法制备了钯纳米颗粒, 然后沉积在Fe3O4/C复合物表面, 得到了不同Fe₃O₄负载量的Pd/Fe₃O₄-C催化剂. 透射电镜（TEM）图显示钯纳米颗粒均匀地分散在Fe₃O₄/C表面. 对制备好的Pd/Fe₃O₄-C催化剂进行了循环伏安法（CV）、计时电流（CA）和电化学阻抗谱（EIS）的测试, 研究了其在碱性介质中对C1-C3醇类（甲醇、乙醇和丙醇）氧化的电催化活性. 结果表明, 所制备的不同Fe₃O₄负载量的Pd/Fe₃O₄(2%)-C,Pd/Fe₃O₄(5%)-C, Pd/Fe₃O₄(10%)-C和Pd/C催化剂中, Pd/Fe₃O₄(5%)-C催化剂表现出最高的醇氧化电流密度. 依据循环伏安（CV）数据,Pd/Fe₃O₄(5%)-C催化剂对甲醇、乙醇、正丙醇和异丙醇氧化的阳极峰电流密度分别是Pd/C催化剂的1.7、1.4、1.7和1.3倍. Pd/Fe₃O₄(5%)-C催化剂对乙醇氧化的电荷传递电阻也远低于Pd/C催化剂. 制备的所有催化剂对C1-C3醇类电氧化的电流密度大小排序如下: 正丙醇﹥乙醇﹥甲醇﹥异丙醇. 此外, 碳粉中Fe₃O₄纳米颗粒的存在提高了钯纳米颗粒的电化学稳定性.     

羧甲基-β-环糊精功能化的四氧化三铁磁性纳米复合物对罗丹明B的吸附性能

基于S_N2取代反应制备了羧甲基-β-环糊精(CM-β-CD),采用层层组装法将其成功修饰在Fe₃O₄磁性纳米粒子表面(MNPs),得到了CM-β-CD功能化的磁性纳米复合物(CM-β-CD-MNPs),通过透射电子显微镜(TEM)、傅里叶变换红外光谱(FTIR)及振动样品磁强计(VSM)等技术手段进行了表征,考察了其对染料罗丹明B(RhB)的吸附性能。 结果表明,CM-β-CD-MNPs呈球形,分散均匀,平均粒径为16 nm,饱和磁化率为54 emu/g,呈超顺磁性。 吸附动力学符合准二级动力学模型,且吸附1 h达到平衡。 吸附等温线符合Langmuir等温吸附模型,最大吸附量为135.1 mg/g。     

纳米Fe2O3和Fe3O4的制备及其催化高氯酸铵热分解性能的研究——一个仪器分析综合实验

介绍一个仪器分析综合实验——纳米Fe_2O_3和Fe_3O_4的制备及其催化高氯酸铵热分解性能的研究。采用水热法合成纳米Fe_3O_4,进而煅烧得到纳米Fe_2O_3。使用X射线粉末衍射(XRD)对制得的样品结构进行表征,通过透射电镜(TEM)可以发现其为球形颗粒,粒径在10–20 nm范围内。将制得的纳米Fe_2O_3和纳米Fe_3O_4按不同比例加入高氯酸铵(AP)中,通过对混合物进行热分析(TG-DSC),发现纳米Fe_2O_3和纳米Fe_3O_4可以明显促进AP的分解,且Fe_2O_3的催化效果优于Fe_3O_4的催化效果,并对催化机理进行了简单讨论。通过该实验,可以让学生学习水热反应的方法,掌握利用XRD、热分析等多种手段对化合物结构及性能进行表征的技能。     

Solid state synthesis and characterization of iron（Ⅱ） pyrophosphate Fe2P2O7

Offwhite pure Fe_2P_2O_7 was synthesized through solid phase reaction using Fe_2O_3 and NH_4H_2PO_4 in argon atmosphere.The reaction products of Fe_2O_3 and NH4_H_2PO_4 at a series of temperatures from 400 to 900℃were characterized by XRD.Comparison and analysis of XRD patterns of resultant products indicated well-crystallized Fe_2P_2O_7 could be obtained over 630℃and Fe_2P_2O_7 prepared at 700℃was triclinic in cell type.Comparison of the cell parameters proved that the as-prepared Fe_2P_2O_7 belonged toβ- Fe_2P_2O_7 in crystal phase and SEM showed its size distribution was 0.5-2μm.     

Design and Preparation of Graphene/Fe2O3 Nanocomposite as Negative Material for Supercapacitor

The development of high specific capacitance electrode materials with high efficiency, scalability and economic feasibility is significant for the application of supercapacitors, however, the synthesis of electrode material still faces huge challenges. Herein, graphene(G)/Fe₂O₃ nanocomposite was prepared via a simple hydrothermal method connected with subsequent thermal reduction process. Scanning electron microscopy(SEM) and transmission electron microscopy(TEM) results showed rod-like Fe₂O₃ nanoparticles were prepared and well-dispersed on graphene layers, providing a rich active site and effectively buffering the aggregation of Fe₂O₃ nanoparticles in the process of electrochemical reaction. The specific capacitance of the obtained G/Fe₂O₃ nanocomposite as negative electrode for supercapacitor was 378.7 F/g at the current density of 1.5 A/g, and the specific capacitance retention was 88.76% after 3000 cycles. Furthermore, the asymmetric supercapacitor(ASC) was fabricated with G/Fe₂O₃ nanocomposite as negative electrode, graphene as positive electrode, which achieved a high energy density of 64.09 W∙h/kg at a power density of 800.01 W/kg, maintained 30.07 W∙h/kg at a power density of 8004.89 W/kg, and retained its initial capacitance by 78.04% after 3000 cycles. The excellent result offered a promising way for the G/Fe₂O₃ nanocomposite to be applied in high energy density storage systems.     

磁性纳米复合物的制备及对铜离子(Ⅱ)的传感检测

采用化学共沉淀法合成硅包覆的磁性纳米粒子Fe_3O_4@SiO_2,进一步通过六亚甲基二异氰酸酯将吡哆酰肼分子(Pyh)接枝到Fe_3O_4@SiO_2表面,制得功能化的磁性纳米复合物(Fe_3O_4@SiO_2-Pyh)。通过傅里叶变换红外光谱、透射电子显微镜、X射线衍射等技术手段对其结构、形貌和磁性能进行了表征。Fe_3O_4@SiO_2-Pyh粒子具有规则的核壳结构,粒径分布在50~55 nm,壳层厚度约为15 nm。Fe_3O_4@SiO_2-Pyh结构中含有酰腙类活性基团—CO—NH—N=CH—,能与Cu~(2+)形成稳定的配合物,在此基础上采用紫外可见吸收光谱特性建立了测定Cu~(2+)的分析方法,线性范围为3.4×10~(-7)~4.5×10~(-6)mol/L,检出限为1.03×10~(-7)mol/L。此外,利用Fe_3O_4@SiO_2-Pyh良好的磁响应,通过外部磁场能够有效地除去水中过量的铜离子,在环境领域具有潜在的应用价值。     

乙基纤维素磁性复合材料对溶液中铜离子的吸附性能

重金属离子对生态环境以及人类健康造成了严重的危害,因此处理水体中的重金属离子迫在眉睫。采用共沉淀法,以乙基纤维素为模版,将四氧化三铁（Fe₃O₄）纳米颗粒与乙基纤维素复合,制备了乙基纤维素磁性复合材料（EC/Fe₃O₄）。探究了吸附添加量、溶液pH值和吸附时间等因素对溶液中Cu（Ⅱ）吸附过程的影响。结果表明,EC/Fe₃O₄表现出良好的吸附速率和吸附性能。吸附4 min,可达到吸附平衡状态。在Cu（Ⅱ）浓度为20 mg/L,pH=7,吸附时间为160 min条件下,EC/Fe₃O₄的单位吸附量q_e为76.98 mg/g,最大去除率为94.68%。在经过8次吸附循环后,单位吸附量为62.21 mg/g。     

Preparation and Properties of Magnetic-fluorescent Microporous Polymer Microspheres

Microporous microspheres can be used as functional nanomaterial carriers for their microporous structure and higher specific surface area. In this study, magnetic fluorescent polymer microspheres were prepared by incorporating Fe₃O₄ nanoparticles and CdSe/ZnS quantum dots(QDs) into hyper-crosslinked microporous polymer microspheres(HCMPs) via the in situ coprecipitation method and swelling-diffusion. The HCMPs predominantly have micropores, and their specific surface area is as high as 703.4 m²/g. The magnetic-fluorescent microspheres maintain the superparamagnetic behavior of Fe₃O₄, and the saturation magnetization reaches 38.6 A·m²/kg. Moreover, the composite microspheres exhibit an intense emission peak at 530 nm and achieve good fluorescence.     

石墨烯量子点磁性复合纳米粒子分散固相微萃取-毛细管电泳法测定肉桂酸及其衍生物

通过一步化学共沉淀法制备了石墨烯量子点(graphene quantum dots,GQDs)包覆的Fe3O4磁性纳米复合材料(Fe3O4-GQDs),并将其用于肉桂酸及其衍生物(肉桂酸、3,4-二甲氧基肉桂酸、4-甲氧基肉桂酸、阿魏酸、反-4-羟基肉桂酸)的固相微萃取,并与毛细管电泳联用建立了测定肉桂酸及其衍生物的新方法。实验考察了吸附溶液的pH值、吸附时间、吸附剂用量、脱附时间等因素对萃取效率的影响。实现了肉桂酸及其衍生物的快速高效富集和高灵敏度检测,加标回收率为86.2%~96.2%,相对标准偏差为1.8%~4.3%。结果表明,合成的Fe3O4-GQDs磁性纳米粒子可作为一种良好的吸附材料应用于特定样品的富集。     

Vc-Functionalized Fe3O4 Nanocomposites as Peroxidase-like Mimetics for H2O2 and Glucose Sensing

A simple and efficient colorimetric biosensing for hydrogen peroxide and glucose with peroxidase-like vitamin C(V_c) functionalized Fe₃O₄ magnetic nanoparticles(V_c/Fe₃O₄MNPs) as a catalyst is reported. Compared with Fe₃O₄ MNPs and other catalysts, V_c/Fe₃O₄ MNPs exhibited superior catalytic properties. Kinetic studies indicated that vitamin C incorporated on Fe₃O₄ MNPs improved the affinity toward H₂O₂. As low as 0.29 μmol/L H₂O₂ can be detected with a wide linear range of 0.5—100 μmol/L H₂O₂; moreover, as low as 0.288 μmol/L glucose can be detected with a linear range of 0.5—25 μmol/L glucose. The detection method was highly sensitive in sensing H₂O₂ and glucose. The robustness of V_c/Fe₃O₄ MNPs rendered them suitable for wide ranging applications.     

Dose-dependent Cytotoxicity and Oxidative Stress Induced by “Naked” Fe3O4 Nanoparticles in Human Hepatocyte

The dose-dependent cytotoxicity effect on human hepatocyte(HL-7702 cells) induced by “naked” Fe3O4 nanoparticles was assessed through cell viabilities and lactate dehydrogenase(LDH) activities. Three important oxidative indexes of the cells by glutathione peroxidase(GSH-Px), superoxide dismutase(SOD) and malondialdehyde( MDA) were determined. The good correlation of the cell viabilities with their GSH-Px, SOD and MDA levels indicated that the cytotoxicity is related to activation of oxidative stress induced by Fe₃O₄ nanoparticles. The oxidative stress also leads to corresponding DNA damage in a similar dose-dependent manner, followed by the changes of cell cycle and cell apoptosis. Such work provides important experimental data for the safety evaluation of superparamagnetic Fe₃O₄ nanoparticles.