反相微乳液法制备纳米Al2O3颗粒及其形成反应机理的研究

通过聚乙二醇辛基苯基醚(曲拉通X-100)/正丁醇/环己烷/水溶液形成的体系, 采用反相微乳液法合成了Al₂O₃纳米粒子. 对前驱体进行热分析(TG-DTG-DTA), 确定了合适的煅烧温度为1150 ℃. 采用X射线衍射(XRD)、透射电镜(TEM)、紫外可见分光光度法(UV-vis)分别对产物的结构、粒度和形貌进行了表征, 考察了微乳液中水与表面活性剂的物质的量之比(ω_o)、煅烧温度和煅烧时升温速率等关键因素对产物形貌和晶相的影响, 并通过分析进一步揭示了Al₂O₃纳米粒子的形成机理. 结果表明, 控制ω_o为10、煅烧温度为1150 ℃可得到分散性好、粒径分布均匀的Al₂O₃纳米粒子, 且2 ℃/min的升温速率更有利于产物向稳定的α晶相转变.     

Efficiency of four different techniques in coupled HPLC-UV/VIS to quantify overlapping peaks with known spectral features

Summary Four different techniques to quantify unresolved chromatographic peaks with known spectral features combined with photodiode array detection, are investigated as regards their efficiency for the accurate and precise determination of drugs in the low g-range. The comparison includes peak suppression utilising difference chromatograms, first-order derivative chromatograms, selective chromatograms, generated by the calculation of orthogonal polynomial shares, and the powerful least-squares multicomponent analysis approach. Each of these methods uses UV-spectra taken throughout, the peak. The results presented and conclusions reached should enable the chromatographer to come to a decision about the reasonable use of these options now provided by multichannel detection in HPLC.     

CdSe纳米线阵列的制备及其表征(英)

通过在含有SeSO₃^2-和Cd²⁺的室温水溶液中，用模板-电沉积法在纳米孔阵列阳极氧化铝膜(AAM)模板中制备了高有序性的CdSe纳米线阵列，并对其形貌、结构和组分进行了表征。扫描电子显微镜(SEM)和透射电子显微镜(TEM)结果表明，纳米线阵列中的CdSe纳米线具有相同的长度和直径，分别对应于使用的AAM模板的厚度和孔径；X-射线衍射(XRD)和X-射线能谱(EDAX)结果表明，CdSe纳米线中Cd和Se的化学组成非常接近于1∶1，其结构为立方CdSe。另外，对模板-电沉积法制备CdSe纳米线的机理进行了讨论。     

四苯硼钠-甲苯胺蓝缔合物纳米微粒体系减色效应研究

在PH4.0醋酸-醋酸钠介质中，甲苯胺蓝在600nm处有一个吸收峰，随着四苯硼钠浓度的增大甲苯胺蓝在600nm处吸收峰降低，颜色减弱，这是由于甲苯胺蓝-四苯硼钠缔合物分子间存在较强的疏水作用及分子间作用力，聚集形成纳米微粒所致，甲苯胺蓝-四苯硼钠纳米微粒体系亦在600mm处有1个吸收峰，在400mm、470mm和580mm处产生3共振散射峰，其中400mm和580mm为甲苯胺蓝-四苯硼钠复合纳米微粒产生的特征共振散射峰，这也表明有纳米微粒存在，丙酮浓度的影响实验结果等表明，纳米微粒的形成是产生其减色效应的原因。     

Target-triggered inhibiting oxidase-mimicking activity of platinum nanoparticles for ultrasensitive colorimetric detection of silver ion

The development of efficient methods for the detection of hazardous and toxic elements is extremely important for environmental security and public health. In this work, we developed a facile colorimetric assaying system for Ag⁺ detection in aqueous solution. Chitosan-stabilized platinum nanoparticles (Ch-PtNPs) were synthesized and severed as an artificial oxidase to catalyze the oxidation of the substrate 3,3′,5,5′-tetramethylbenzidine (TMB) and generate color signal. In the presence of Ag⁺, due to the strong metallophilic interactions between Ag⁺ and Pt²⁺ on the surface of Ch-PtNPs, Ag⁺ can weaken the affinity to the substrates and inactivate the catalytic activity of Ch-PtNPs, leading to decreased absorbance signal to varying degrees depending on Ag⁺ amount. Combing the specific binding between Ch-PtNPs and Ag⁺ with signal amplification procedure based on the Ch-PtNPs-catalyzed TMB oxidation, a sensitive, selective, simple, cost-effective, and rapid detection method for Ag⁺ can be realized. Ag⁺ ions in tap and lake waters have been successfully detected. We ensured that the proposed method can be a potential alternative for Ag⁺ determination in environmental samples.     

High-performance liquid chromatographic determination of Levetiracetam in human plasma: comparison of different sample clean-up procedures

An accurate and precise high-performance liquid chromatographic method using diode array detection for the determination of the novel antiepileptic, Levetiracetam, has been developed. Three clean-up procedures for the analysis of Levetiracetam in human plasma were implemented and evaluated, namely solid-phase extraction, deproteinization by addition of organic solvents and formation of insoluble salts. Adenosine was used as the internal standard for all three sample pretreatment procedures. Among the several cartridges used for solid-phase extraction, the hydrophilic-lypophilic balance (Oasis) HLB) phase provides the best extraction yield of Levetiracetam, together with high precision. With the two other clean-up procedures involving plasma deproteinization by addition of methanol or zinc sulphate, lower sensitivity and precision of the assays were obtained. However, they are cheaper and faster when compared with the solid-phase extraction procedure.     

Gold nanoparticle-enhanced surface plasmon resonance measurement with a highly sensitive quantification for human tissue inhibitor of metalloproteinases-2

Two different methods for the quantification of human tissue inhibitor of metalloproteinases-2 (TIMP-2) were developed using surface plasmon resonance (SPR) and gold nanoparticles for signal enhancement. The first method, a competitive assay, used TIMP-2 immobilized to the sensor surface and the inactive form of matrix metalloproteinase-2 (proMMP-2) (EC 3.4.24.24) adsorbed to gold nanoparticles. The sensor signals resulting from the interaction of MMP-2-gold nanoparticles with immobilized TIMP-2 were inversely proportional to the amounts of TIMP-2 of the sample. The measuring range for TIMP-2 was about 15–180 pM. The second method, a one-step sandwich assay, used proMMP-2 immobilized to the sensor surface and an anti-TIMP-2 monoclonal antibody coupled to gold nanoparticles. The lower detection limit of this assay format was 0.5 pM of TIMP-2. The binding signals were highly reproducible up to 100 pM of the inhibitor. The improvements obtained in TIMP-2 quantification over already existing tests could contribute to a better understanding and diagnosis of diseases like cancer.     

HPLC quantification of flavonoids and biflavonoids inCupressaceae leaves

Summary The aim of this investigation was to obtain qualitative and quantitative profiles of the flavonoid and biflavonoid composition of six cypress species—Cupressus funebris L.,Cupressus sempervirens L.,Cupressus glabra L.,Cupressus arizonica L.,Cupressus goveniana L., andCupressus lusitanica L. HPLC-diode-array detection (DAD), HPLC-MS, and HPTLC were used to identify the individual compounds. A chromatographic method was optimized for identification and quantification of the main flavonoid glycosides and biflavonoids. The flavonoids identified and calibrated were: rutin, quercetin glucoside, quercetin rhamnoside, and kaempferol 3-O-rhamnoside. The biflavonoids identified and calibrated were: cupressuflavone, amentoflavone, robustaflavone, hinokiflavone, methylrobustaflavone, methylamentoflavone, and dimethylcupressuflavone.     

N-TiO2/ZnO复合纳米管阵列的掺杂机理及其光催化活性

以ZnO纳米柱阵列为模板, 采用溶胶-凝胶法制备出TiO2/ZnO和N掺杂TiO2/ZnO的复合纳米管阵列. 扫描电镜(SEM)、X射线光电子能谱(XPS)和紫外-可见漫反射吸收光谱(UV-Vis)的结果表明: 两种阵列的纳米管均为六角形结构, 直径约为100 nm, 壁厚约为20 nm; 在N-TiO2/ZnO复合纳米管阵列中, 掺入的N离子主要是以N-Ox、N-C和N-N的形式化学吸附在纳米管表面, 仅有少量的N离子以取代式掺杂的方式占据TiO2晶格O的位置; 表面N物种形成的表面态能级和取代式掺杂导致带隙的窄化, 增强了纳米管阵列的光吸收效率, 促进了光生载流子的分离. 光催化实验结果表明, N离子的掺杂有利于N-TiO2/ZnO复合纳米管阵列光催化活性的提高.