组合电化学--电化学研究中的新策略

组合电化学是一种新的电化学研究策略，通过设计和构建大量多样性的电极阵列，并对其进行高通量筛选和表征，快速、高效地实现了体系的电化学研究。本文综述了近年来进行的组合电化学研究，重点介绍了组合光学筛选方法、组合电化学合成方法以及电化学平行筛选方法，并探讨了各种方法的优势和存在的问题。     

Preparation of Silver Nanoparticles through Alcohol Reduction with Organoalkoxysilanes

Silver nanoparticles of narrow size distribution were prepared through the chemical reduction in an alcohol solution with several organoalkoxysilanes. In this system, organoalkoxysilanes served as a stabilizer, protecting silver nanoparticles from aggregation. The changes in size and morphology of colloidal silver nanoparticles were investigated with the addition of organoalkoxysilanes such as 3-aminopropyltriethoxysilane (APS), methyltriethoxysilane (MTS), phenyltrimethoxysilane (PTS), vinyltriethoxysilane (VTS), and 3-glycidoxypropyltrimethoxysilane (GPS) as stabilizers. The organic functional groups of organoalkoxysilanes interact with silver ions and clusters, which stabilize silver nanoparticles in the system. The silver nanoparticles obtained were characterized with transmission electron microscopy (TEM), UV-vis spectroscopy, etc.     

一种N-酰肌氨酸在四氧化三铁纳米颗粒表面的吸附特征

根据表面活性剂固液界面吸附理论和表面改性颗粒亲水疏水特性及红外光谱分析,提出了不同四条件和表面活性剂用量下不同的吸附模型。     

Studies of poly-<Emphasis Type="Italic">L</Emphasis>-lysine-starch nanoparticle preparation and its application as gene carrier

Anion starch nanoparticle (StNP) with a diameter of 50 nm was prepared in water-in-oil microemulsion, with soluble starch as raw materials and POCl₃ as crosslinking agent. PLL-StNP was prepared by linking poly-L-lysine (PLL) on the surface of StNP. At the same time, the size of PLL-StNP and its stability in aqueous solution were checked by AFM. The analysis of plasmid DNA binding, DNase I enzymatic degradation, toxicity and transfection were done. We discovered that PLL-StNP may be used as non-virus nanoparticle gene carrier. And we developed the method of preparing PLL-StNP gene carrier and used it in cell transfection. As non-virus gene carrier, PLL-StNP has some advantages, such as large load of DNA, high transfection efficiency, low cell toxicity and biodegradability.     

Tests for liquid chromatographs

Summary The paper describes tests for liquid chromatographs to assess the autosampler and pump flow rate precision; suitability of the instrument for normal phase chromatography; UV detector performance; and external band broadening characteristics. Tests for mixing and proportioning characteristics of solvent pumps and performance of diode array detectors are also considered. These tests are designed to evaluate the performance of both newly released liquid chromatography equipment and equipment already in operation. Data from evaluations carried out by instrument manufacturer’s and suppliers is reported and discussed. This data offers specifications to a common format for initial selection of instruments prior to purchase.     

Contribution of dimensional factor to the potential of copper-containing electron-ion exchangers

The average size of copper particles in copper-containing electron-ion exchangers is determined with the aid of microscopy and x-ray diffractometry. The results are used to calculate the contribution made by a dimensional factor to the electrode potential. Compared to the potential of compact copper, the potential shift in the negative direction measured experimentally falls within the region of calculated values. The average size of copper particles remains practically unchanged after contact with a copper sulfate solution, testifying to stabilization of an ultradisperse state of copper particles by a polymer matrix.     

氨水溶液制备ZnO纳米晶阵列的研究

以氨水和硝酸锌为前躯体，采用低温水溶液法在涂敷ZnO晶种层的玻璃衬底上外延生长了ZnO纳米棒晶阵列。应用SEM、TEM、SAED和XRD表征了ZnO纳米晶的形貌和结构。讨论了该组成体系水溶液法纳米棒外延生长的机理及其对棒晶形貌的影响。通过对水溶液pH值的原位二次调整，制备出了ZnO纳米管和表面绒毛状的棒晶阵列，基于生长机理探讨了它们的形成原因，为实现不同形貌ZnO纳米晶阵列的优化控制提供了可能的技术途径。结果表明，不同形貌的ZnO均属沿c轴择优取向的六方纤锌矿结构。     

Trace Detection of Mercury(II) Using Gold Ultra‐Microelectrode Arrays

The electroanalytical detection of trace mercury(II) at gold ultra‐microelectrode arrays is reported. The arrays consist of 256 gold microelectrodes of 5 μm in diameter in cubic arrangements which are separated from their nearest neighbor by 100 μm. The array was utilized in nitric acid using linear sweep voltammetry where a linear response from mercury additions over the range 10 μg L^?1?200 μg L^?1 (10^?8?10^?6 M) was observed with a sensitivity and detection limit of 0.11 nC/μg L^?1 and 3.2 μg L^?1 (16 nM) respectively from using a deposition time of 30 s at ?0.2 V (vs. SCE). This methodology was explored in 0.1 and 1 M chloride media over the mercury range 10 μg L^?1?200 μg L^?1 (5×10^?8?10^?6 M) where similar sensitivities of 0.087 nC/μg L^?1 and 0.078 nC/μg L^?1 were observed with an identical detection limit. The protocol is demonstrated to be useful for the determination of mercury for analysis of environmental water samples.     

Simplified Solid-Phase Extraction Procedure and Liquid Chromatographic Determination of Celecoxib in Rat Serum

A simplified solid phase extraction method, eliminating a preliminary protein precipitation has been developed for the determination of celecoxib in rat plasma. The technique included a solid phase extraction of the serum samples on a [poly (divinylbenzene-co-N-vinylpyrrolidone)] sorbent. After conditioning, the cartridge was loaded with 0.5 mL of acidified serum containing internal standard. Elution was made with 1 mL of a mixture of acetonitrile and methanol (1/1, v/v). After evaporation of the eluate to dryness and reconstitution with methanol, the samples were analyzed on an octadecyl bonded phase with several mobile phases containing acetonitrile and a phosphate buffer. Detection was carried out using a Photodiode Array Detector. Full validation of the proposed method was provided (linearity range: 0.01–2 mg. L^–1, average extraction efficiency: 92.4%; average intra-day variability: 4.6% with an accuracy of 94.8%; average interday variability: 5% with an accuracy of 95.3%, limit of detection: 0.005 mg. L^–1, limit of quantification: 0.002 mg. L^–1). The proposed method was successfully utilised to quantify celecoxib in rat plasma for a pharmacokinetic study.Revised: 26 January and 23 April 2004     

Microdevices for manipulation and accumulation of micro- and nanoparticles by dielectrophoresis

Microfluidic devices with three-dimensional (3-D) arrays of microelectrodes embedded in microchannels have been developed to study dielectrophoretic forces acting on synthetic micro- and nanoparticles. In particular, so-called deflector structures were used to separate particles according to their size and to enable accumulation of a fraction of interest into a small sample volume for further analysis. Particle velocity within the microchannels was measured by video microscopy and the hydrodynamic friction forces exerted on deflected particles were determined according to Stokes law. These results lead to an absolute measure of the dielectrophoretic forces and allowed for a quantitative test of the underlying theory. In summary, the influence of channel height, particle size, buffer composition, electric field, strength and frequency on the dielectrophoretic force and the effectiveness of dielectrophoretic deflection structures were determined. For this purpose, microfluidic devices have been developed comprising pairs of electrodes extending into fluid channels on both top and bottom side of the microfluidic channels. Electrodes were aligned under angles varying from 0 to 75 degrees with respect to the direction of flow. Devices with channel height varying between 5 and 50 microm were manufactured. Fabrication involved a dedicated bonding technology using a mask aligner and UV-curing adhesive. Particles with radius ranging from 250 nm to 12 microm were injected into the channels using aqueous buffer solutions.