室温离子液体中金纳米粒子的电化学制备及其表征

室温离子液体1乙基3甲基咪唑四氟硼酸盐中,采用电化学牺牲阳极法直接从金属金制备了球形金纳米粒子,采用X射线衍射（XRD）、带有电子能谱仪（EDS）的扫描电子显微镜（SEM）对所制备样品的结构、组成以及形态进行了表征.结果表明,在本实验条件下制得的金纳米粒子为面心立方结构,纯度较高,基本呈球形,粒径平均尺寸为20nm.     

毛细管胶束电动色谱分离测定对硫磷、甲基对硫磷、水胺硫磷和克百威

用毛细管胶束电动色谱成功地分离 4种农药对硫磷、甲基对硫磷、水胺硫磷和克百威 .研究了电泳缓冲液的pH、浓度、及表面活性剂浓度等影响因素 ,在选定的最佳分离条件pH7.4、2 0mmol L硼酸 -四硼酸钠缓冲液 +30mmol LSDS下 ,4组份在 9min内得到基线分离 .检测限分别为 :对硫磷 2 .0 μg mL、甲基对硫磷 1.8μg mL、水胺硫磷 0 .8μg mL及克百威 1.0 μg mL .该方法成功地应用于模拟土壤样品中农药残余物的测定 ,回收率为 97.0 % - 10 3.8% .     

基于金纳米通道分离检测百草枯与阿特拉津

利用化学沉积法在聚碳酸酯膜上沉积金,得到的金纳米通道表面带有负电荷,具有亲水性.阿特拉津和百草枯在结构性质上存在差异,百草枯为亲水性分子,水溶液中以阳离子形式存在,而阿特拉津为疏水性分子,水溶液中以分子形式存在,在外加电场的条件下,离子型百草枯由于电泳的作用会发生定向迁移,利用这一特点,实现对两者分子的分离.     

毛细管电泳分离DNA片段的研究

以羟丙甲基纤维素作为筛分介质，３７ｃｍ×７５μｍ涂层石英毛细管，在 ７ ｋｖ电压下，毛细管电泳分离了 φ１７４ ＤＮＡ／ＨａｅⅢ Ｍａｒｋｅｒｓ．     

Two-dimensional self-organization of 1-nonanethiol-capped gold nanoparticles

A two-dimensional (2D) ordered hexagonal close-packed structure, formed by 1-nonanethiol-capped gold nanoparticles, is reported. The structure was constructed only by dipping the gold nanoparticle colloidal solution on flat substrate. The gold nanoparticles were synthesized as follows: First, AuCl₄^-1 was transferred from aqueous solution to toluene by the phase-transfer reagent of tetraoctylammonium bromide. Then it was reduced with aqueous sodium borohydride in the presence of a given amount of 1-nonanethiol molecules which was used to control the nucleation and growth of the gold nanoparticles for the desired size. The experimental techniques, such as UV-Vis, FT-IR, and X-ray photoelectron spectroscopy (XPS), were employed to characterize the obtained product. Transmission electron microscopy (TEM) measurement demonstrated the size of the gold nanoparticle and the formation of two-dimensional ordered hexagonal close-packed gold nanoparticle structure.     

纳米金溶液中表面增强红外研究

基于衰减全反射模式下的表面增强红外,已广泛用于界面吸附的研究.作者报道一种基于外反射模式下的表面增强红外光谱电化学技术.在纳米金溶液中,研究了多巴胺和钴-邻菲罗啉配合物的光谱电化学行为.研究表明,吸附在均匀分散于水溶液中纳米金颗粒的多巴胺和钴-邻菲罗啉配合物分子,能够表现出显著的红外增强现象.这种现象是由于带正电荷的多巴胺和钴-邻菲罗啉配合物由于静电作用吸附至带负电性的纳米金颗粒表面,从而表现出红外吸收增强现象.     

基于Au纳米通道膜分离大豆异黄酮单体的研究

以聚碳酸酯滤膜为模板,采用化学沉积法将Au沉积到膜孔道内,制备了直径约10nm的Au纳米通道膜（Au．Mem）,对巯基苯胺（PATP）通过金一硫键共价自组装至Au纳米通道孔壁上,形成致密单层氨基末端的Au纳米通道膜（PATP—Au—Mem）,pATP末端氨基在较低pH值条件下易被质子化而使Au纳米通道膜带正电荷,对于荷正电的物质通过纳米通道膜具有静电斥力作用．利用染料木素与铝可形成荷正电的螯合物后不易通过Au纳米通道的特性,在pH=4．5的条件下,基于PATP。Mem膜分离了大豆异黄酮单体染料木素与大豆黄素,其分离度可达6．91．     

表面修饰的金纳米粒子的制作及表征

通过硼氢化钠NaBH4还原金氯酸HAuCl4，成功地制作了羧酸酯表面修饰的金纳米粒子，并用丁二酸硫醇作为硫醇配体稳定剂，抑制了纳米粒子的进一步生长，这种方法有效地把粒径控制在纳米范围内并且粒径分布范围小，只需通过一次反应就可大量地制得1－20nm、具有量子效应的纳米料，用X射线衍射仪、透射式电子显微镜和隧道扫描显微镜对这些粒子进行了检测，证实了大量的粒子都是面心立方结构，硫醇配体在金粒子在表面由化学吸附形成一层单分子膜，隧道扫描显微镜观察到了这一层单分子膜。     

双键功能化的金纳米粒子的制备与表征

通过四辛基溴化铵稳定的金纳米粒子(TOAB-Au)与含可聚合双键的二硫化物配体之间的置换反应,制备了四种双键功能化的金纳米粒子,并通过紫外光谱、红外光谱、X-光电子能谱、透射电镜和热重分析对金纳米粒子的形貌和组成进行了表征。结果表明,双键功能化的金纳米粒子能够稳定地分散在氯仿和四氢呋喃溶剂中,粒子直径在4 nm到8 nm之间,表面等离子共振吸收峰随配体的不同在521 nm到532 nm之间改变。四种双键功能化的金纳米粒子的表面配体接枝密度在4.2到6.6之间。     

纳米金修饰电极和探针载体的DNA电化学发光分析方法研究

提出以纳米金修饰电极和以纳米金粒子作DNA探针载体的电化学发光检测DNA新方法.首先将纳米金自组装在金电极上,再将含巯基的目标ss-DNA固定于纳米金修饰的电极上,然后与以纳米金粒子作载体的电化学发光DNA探针进行杂交反应,将此电极做工作电极,在含有三丙胺的溶液中进行电化学发光测量.在选定实验条件下,检测囊肿纤维DNA片断(20 base)的线性范围为1.0×10-12~1.0×10-9mol/L,相关系数为0.9954,检出限为5.0×10-13mol/L.实验结果表明,纳米金具有较大的比表面积,可增强DNA在电极上的固定量,从而增强电化学发光检测信号,提高方法的灵敏度.     

不同制备因素对纳米金尺寸的影响

通过化学还原法制备出不同粒径的纳米金(GNPs).利用紫外-可见分光光度计(UVVis)和透射电子显微镜(TEM)对GNPs的形貌及尺寸进行表征.讨论了还原剂种类、还原剂用量、保护剂等因素对GNPs形貌、粒径、稳定性和分散性的影响.结果表明:还原剂柠檬酸钠的用量直接影响GNPs的尺寸大小,但当柠檬酸钠用量超过3 mL时,制得GNPs的尺寸不再变化,以柠檬酸钠为还原剂制得GNPs粒径在13~50 nm之间,分散性好且尺寸较均匀,此时,保护剂PVP对大尺寸GNPs的制备影响不大;以硼氢化钠为还原剂,可制得GNPs粒径在2~3 nm之间,分散性好,此时保护剂PVP对于制备的影响较显著,但不影响GNPs的可控制备.     

High-conductivity graphene nanocomposite via facile, covalent linkage of gold nanoparticles to graphene oxide

Graphene and its derivative,graphene oxide (GO) have been substantively used as the main framework for dispersing or building nanoarchitectures because of their excellent properties in electronics and catalysis.The requirement to obtain superior graphene-metal hybrid nanomaterials has led us to explore a facile way to design 4-aminobenzenethiol/1-hexanethiolate-protected gold nanoparticles (aAuNPs)-functionalized graphene oxide composite (aAuNPs-GO) in solution.We demonstrate that when aAuNPs with amino groups are exposed to GO,well-dispersed coverage of Au nanoparticles are mainly observed on the edge of GO sheet.In contrast,when 1-hexanethiolate-protected gold nanoparticles (hAuNPs) without amino groups are exposed to GO,hAuNPs simply aggregate on the surface of GO.This indicates that amino groups located on the surface of Au nanoparticles are an essential prerequisite for attachment of nearly monodispersed aAuNPs.The strategy described here for the fabrication of aAuNPs-GO provides a straightforward approach to develop graphene-based nanocomposites with undamaged sheets structure and good solubility and also improve the conductivity of GO sheets evidently.     

金纳米粒子修饰电极上电化学发光法测定二茂铁羧酸的研究

在金纳米粒子修饰石墨电极上,鲁米诺-过氧化氢-二茂铁羧酸体系的电化学发光有增敏作用.详细考察了在金纳米粒子修饰石墨电极上鲁米诺-过氧化氢-二茂铁羧酸体系的电化学发光行为,研究了影响发光信号的多种因素,优化了测定二茂铁羧酸的分析条件.结果表明,在2.5×10-9mol/L鲁米诺,1.0×10-3mol/L过氧化氢,0.10 mol/L pH值为9.2碳酸氢钠缓冲溶液中,以金纳米粒子修饰石墨电极为工作电极,控制电位为 390 mV,二茂铁羧酸浓度在1.0×10-9~1.0×10-6mol/L范围内与电化学发光强度呈良好的线性响应关系,检出限为7×10-10mol/L(S/N=3).     

抗生素的毛细管电泳分离

通过对电极缓冲体系、pH值、乙腈添加浓度、N -甲基吗啡啉添加浓度及温度、电压的优化选择 ,用毛细管电泳方法分离土霉素、金霉素、多西环素、四环素、氯霉素 5种抗生素 .应用胺类修饰剂N -甲基吗啡啉作为添加剂 ,提高了抗生素的分离效果 .实验结果表明 ,此方法操作简单快速、成本低、定量准确 (R <0 .9917)、灵敏度高 ,检测极限分别为 0 .0 118,0 .0 2 36 ,0 .0 118,0 .0 118,0 .0 0 0 4ng .     

正常红细胞与异常红细胞的毛细管电泳分离

通过对红细胞的毛细管电泳行为的研究,建立了利用毛细管电泳检测鉴定红细胞不同状态的方法,在含6%葡萄糖的磷酸盐缓冲液(0.1 mol/L pH 7.4),(50 cm/65 cm)×75μm毛细管,进样5 s,电压20 kV,温度25℃的电泳条件下可获得尖锐且对称的细胞峰;同时,成功分离了正常红细胞和被病毒感染的异常红细胞,分离度达1.04,并在此基础上考察不同损伤程度的红细胞的泳动行为.     

Nanostructured multilayer thin films of multiwalled carbon nanotubes/gold nanoparticles/glutathione for the electrochemical detection of dopamine

In the present study, multiwalled carbon nanotubes (MWCNTs), gold nanoparticles (AuNPs), and glutathione (GSH) were used to fabricate multilayer nanoscale thin films. The composite thin films were fabricated by layer-by-layer technique as the films were constructed by the alternate deposition of cationic and anionic polyelectrolytes. The MWCNTs were modified via a noncovalent surface modification method using poly(diallydimethylammonium chloride) to form a cationic polyelectrolyte. An anionic polyelectrolyte was prepared by the chemical reduction of HAuCl4 using sodium citrate as both the stabilizing and reducing agent to form anionic AuNPs. GSH was used as an electrocatalyst toward the electro-oxidation of dopamine. The constructed composite electrode exhibits excellent electrocatalytic activity toward dopamine with a short response time and a wide linear range from 1 to 100 μmol/L. The limits of detection and quantitation of dopamine are (0.316±0.081) μmol/L and (1.054±0.081) μmol/L, respectively. The method is satisfactorily applied for the determination of dopamine in plasma and urine samples to obtain the recovery in the range from 97.90% to 105.00%.     

异丙嗪旋光异构体的毛细管区带电泳分离

研究用不同的手性选择剂拆分异丙嗪旋光异构体。用手细管区带电泳法拆分异丙嗪旋光异构体。研究表明,用低浓度β－环糊精（β－ＣＤ）可基线分离异丙嗪旋光异构体,用谷氨酸－β－ＣＤ不能基线分离,而用由两者组成的混合手性剂体系所造成的分离介于用各单个手性选择剂所造成的分离选择性之间,在一些混合比例下也可其线分离异丙嗪旋光异构体。手性选择剂的种类和浓度对分离结果有较大影响。     

纳米粒子应用于微生物检测的研究进展

食源性致病菌是引发食源性疾病的主要因素,如何有效地检测出食源性致病菌的存在是食源性疾病预防与控制的关键环节.目前,应用于食源性致病菌检测领域的纳米粒子技术已日益成熟.系统介绍了光学纳米粒子、磁性纳米粒子等技术在微生物致病菌检测中的应用.     

毛细管电泳-安培检测法同时测定白藜芦醇及虎杖甙

采用毛细管电泳-电化学检测技术(CE-ECD)对白藜芦醇及虎杖甙进行分离检测.采用柱端喷壁式安培检测方式,在最佳分离条件下,2待测物在12 m in以内完全分离.白藜芦醇和虎杖甙分别在1.2×10-6~1.0×10-4mol/L与6.0×10-7~5.0×10-5mol/L浓度范围内与峰电流成良好的线性关系,检测下限分别为1.6×10-7和2.3×10-7mol/L.将该体系用于中药虎杖、中成药护肝宁片及市售红葡萄酒的分析和回收实验,测定结果令人满意.