An efficient and facile synthesis of inhibitors for hepatitis C viral and anti-SARS agents: 4-aryl-5-cyano-1,6-dihydro-2-thiouracils

One-pot, multicomponent reaction for the synthesis of 4-aryl-5-cyano-1,6-dihydro-2-thiouracils via three-component from aromatic aldehydes, ethyl 2-cyanoacetate and S-benzylisothiourea hydrochloride (methyl carbamimidothioate sulfate) under methanol is described. These compounds have many drug activities, such as anti-hepatitis C viral, anti-Severe acute respiratory syndrome and anti-HIV-1 integrese activity. The advantages of this procedure include the short reaction time, mild reaction conditions and excellent yields.     

A magnetic copper(II)-imprinted polymer for the selective enrichment of trace copper(II) ions in environmental water

We have developed a convenient, selective and reliable method for the rapid enrichment of trace quantities of Cu(II) by using a magnetic Cu(II) ion-imprinted polymer. This is followed by their determination by FAAS. The imprints were prepared by using (a) Cu(II) ions as the template, (b) 3-aminopropyltriethoxysilane as both the functional monomer and the crosslinking agent, and (c) Fe₃O₄ as the magnetic component. Enrichment is carried out in a single step, and adsorbed copper ions can be separated from the sample solution by applying a strong magnet. The effects of pH, elution condition, amount of imprint, and of potentially interfering ions were evaluated. Under the optimal conditions, the detection limit and enrichment factor are 0.3?μg L^?1 and 100, respectively, and the recovery is >95?%. The procedure was successfully applied in the enrichment and detection of trace copper ions in environmental water.

Thermal transformation of δ-MnO2 nanoflowers studied by in-situ TEM

In-situ transmission electron microscopy in combination with a heating stage has been employed to real-time monitor variations of -phase MnO2 nanoflowers in terms of their morphology and crystalline structures upon thermal annealing at elevated temperatures up to ~665℃. High-temperature annealing drives the diffusion of the small δ-MnO2 nanocrystallites within short distances less than 15 nm and the fusion of the adjacent δ-MnO2 nanocrystallites, leading to the formation of larger crystalline domains including highly crystalline nanorods. The annealed nanoflowers remain their overall flower-like morphology while they are converted to δ-MnO2 . The preferred transformation of the δ-MnO2 to the δ-MnO2 can be ascribed to the close lattice spacing of most crystalline lattices between δ-MnO2 and δ-MnO2 , that might lead to a possible epitaxial growth of δ-MnO2 lattices on the δ-MnO2 lattices during the thermal annealing process.     

ZnNe低激发态的量子化学研究

用相对论赝势ＣＡＳＳＣＦ／ＣＩ方法,对ＺｎＮｅ的基态和低激发态进行了计算,得出了它们的电子结构,势能曲线及光谱常数。计算结果表明,ＺｎＮｅ的基态分子是范德华分子,它的几个低激发态分子中的主要作用力为范德华力,这些态的分子仍为范德华分子。     

Separation and characterization of sucrose esters from Oriental tobacco leaves using accelerated solvent extraction followed by SPE coupled to HPLC with ion‐trap MS detection

Sucrose esters (SEs) were successfully extracted from Oriental tobacco leaves using a new methodology based on accelerated solvent extraction followed by hydrophilic–lipophilic balanced cartridge cleanup step. The SEs were detected by HPLC with ion‐trap MS detection using an electrospray interface operated in the positive ion mode. This methodology combines the high efficiency of extraction provided by a pressurized fluid and the highly sensitive characterization offered by ion‐trap MS. Under the optimized conditions, 14 SEs were first identified among a total of 23 SEs found in Oriental tobacco leaves. Under the same conditions, only four new SEs were extracted by using traditional ultrasound‐assisted extraction and liquid–solid extraction methods. The present method might be potentially useful in high‐efficiency extraction and sensitive characterization of SEs from complex matrices such as tobacco leaves.     

Direct determination of chlorophenols in water samples through ultrasound-assisted hollow fiber liquid–liquid–liquid microextraction on-line coupled with high-performance liquid chromatography

In this study we on-line coupled hollow fiber liquid–liquid–liquid microextraction (HF-LLLME), assisted by an ultrasonic probe, with high-performance liquid chromatography (HPLC). In this approach, the target analytes – 2-chlorophenol (2-CP), 3-chlorophenol (3-CP), 2,6-dichlorophenol (2,6-DCP), and 3,4-dichlorophenol (3,4-DCP) – were extracted into a hollow fiber (HF) supported liquid membrane (SLM) and then back-extracted into the acceptor solution in the lumen of the HF. Next, the acceptor solution was withdrawn on-line into the HPLC sample loop connected to the HF and then injected directly into the HPLC system for analysis. We found that the chlorophenols (CPs) could diffuse quickly through two sequential extraction interfaces – the donor phase – SLM and the SLM – acceptor phase – under the assistance of an ultrasonic probe. Ultrasonication provided effective mixing of the extracted boundary layers with the bulk of the sample and it increased the driving forces for mass transfer, thereby enhancing the extraction kinetics and leading to rapid enrichment of the target analytes. We studied the effects of various parameters on the extraction efficiency, viz. the nature of the SLM and acceptor phase, the compositions of the donor and acceptor phases, the fiber length, the stirring rate, the ion strength, the sample temperature, the sonication conditions, and the perfusion flow rate. This on-line extraction method exhibited linearity (r² ≥ 0.998), sensitivity (limits of detection: 0.03–0.05 μg L⁻¹), and precision (RSD% ≤ 4.8), allowing the sensitive, simple, and rapid determination of CPs in aqueous solutions and water samples with a sampling time of just 2 min.     

Facile One-Pot,Multicomponent Synthesis of Pyridines Under Microwave Irradiation

A series of 2-amino-6-(2-oxo-2H-chromen-3-yl)-4-pyridine-3-carbo-nitriles were synthesized by the one-pot, multicomponent reaction of 3-acetyl-coumarin, aromatic aldehydes, malononitrile, and ammonium acetate in acetic acid under microwave irradiation. The reactions were completed in 10–13 min with 61–86% yields, were environmental benign, and had easy workup. Their structures were confirmed by ¹H NMR, IR, and MS spectra and elemental analysis.     

稀土单氧化物发射光谱法的研究I.混合稀土浓集物中钐的双波长测定

报道了空气乙炔火焰中ＳｍＯ蒸气的发射光谱行为，试验了Ｌａ、Ｎｄ、Ｅｕ、Ｙ对ＳｍＯ发射强度增强作用，在大量Ｌａ存在下，ＳｍＯ的发射强度与其浓度成正比关系。用大量Ｌａ作增感剂和干扰抑制剂，借助双波长测定法克服光谱干扰，实现了直接测定高Ｙ混合稀土浓集物中的Ｓｍ，方法准确，快速     

亚甲蓝作为酶电极电子传递介体的性能研究

研究了亚甲蓝修饰的玻碳电极的催化性能，并以此电极为基础电极研制了介体修饰型多酚氧化酶电极，对多巴胺测定的检出限为５×１０－６ｍｏｌ／Ｌ，较空白电极降低了４００倍，而对维生素Ｃ的响应则显著减小，其电流值降低至空白电极的十分之一．因此不仅显著提高了灵敏度，选择性也得到很大的改善．