Determination of Enantiomeric Excess of Glutamic Acids by Lab-made Capillary Array Electrophoresis

The techniques of combinatorial chemistry have recently been applied to the discovery of new asymmetric catalyst for a variety of organic transformations1-3. Using combina- torial methods, it is straightforward to generate thousands of potential asymmetri…     

端视式全谱直读电感耦合等离子体发射光谱法测定高纯氧化镧中稀土杂质

电感耦合等离子体发射光谱(ICP-AES)测定高纯氧化镧中14个稀土元素杂质,镧对其它稀土元素的光谱干扰比较严重,要求光谱仪单色器有较高的分辨率。使用端视式全谱直读ICP-AES仪,选择测定波长,工作参数优化,讨论了镧和酸度的影响。大部分稀土元素测定使用曲线拟合(FACT)的背景校正方法。该方法的稀土元素氧化物检出限达到3×10-4~0.022 mg.L-1(3σ)。     

Applications of a miniaturized fluorimetric photodiode array detector for capillary liquid chromatography

A high sensitivity, multichannel fluorescence detector with small volume has been developed for capillary column liquid chromatography. Using an intensified linear photodiode array to monitor fluorescence emission, several important mixtures exhibiting native fluorescence have been examined following high efficiency separation on a capillary column. By correlating mass spectral, fluorescence spectral, and retention time data, information of potential utility in the structural elucidation of aromatic molecules contained in complex mixtures can be obtained. Examples include the separation and spectral examination of the polyaromatic compounds in samples of both biological and environmental interest.     

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.     

碱性水蒸气处理的ZSM-5沸石酸性质及孔结构的影响

 采用XRD，NH3－TPD，比表面积和孔结构测定等研究了在不同温度下用含10％NH3的水蒸气处理时HZSM－5沸石n（Si）／n（Al）＝25）酸性质及孔结构的变化规律．结果表明，随着处理温度的提高，HZSM－5的结构未发生明显的变化；样品的总酸量下降很快，但弱酸分布量相对提高，而强酸分布量相对下降；提高处理温度，样品的比表面积和微孔体积减小，二次孔或中孔体积及外表面积有增大的趋势．     

高比表面积窄孔分布氧化铝的制备研究 Ⅰ.沉淀条件的影响

 以硫酸铝液为原料，以氨水、氢氧化钠和铝酸钠为碱沉淀剂，采用pH摆动法制备了高比表面积、大孔径、窄孔分布、大孔体积氧化铝，考察了沉淀剂、沉淀温度及沉淀时酸侧pH值对氧化铝物性的影响，并对pH摆动法与等pH沉淀法的结果进行了比较．结果表明，通过改变制备参数可以获得高比表面积、大孔体积的氧化铝，当沉淀温度为70℃，pH摆动3或4次时，氧化铝的孔体积可高达1．0ml／g，比表面积仍大于300m2／g．用pH摆动法制得的样品比用等pH沉淀法制得的样品容易酸溶，对挤压成型有利．不同样品在酸溶液中的分散性表明，用氨水沉淀剂可获得相对较小的沉淀粒子．改变沉淀时酸侧的pH值，可导致沉淀粒子的结构发生变化．     

Fermentation characteristics and the dynamic trend of chemical components during fermentation of Massa Medicata Fermentata

As a representative of traditionally fermented Chinese medicine, Massa Medicata Fermentata (MMF) shows the functions of invigorating the spleen and stomach and promoting digestion, which plays an important role in the treatment of gastrointestinal diseases. The fermentation mechanism and the key factors that affect the quality of MMF have not been revealed yet, which has become an urgent issue that limits its clinical application. This article aims to systematically and comprehensively reveal the transformation of physical properties and the dynamic trend of chemical components including substrate components, volatile components, and lactic acid as anaerobic fermentation product during MMF fermentation. Along with obvious hyphae growth observed for MMF, the weight of MMF decreased, and the moisture and temperature increased. Through the quantified 14 components from substrate, ferulic acid increased from 45.53 ± 6.94 to 141.89 ± 78.40 μg/g, while glycosides and phenolic acids declined except caffeic acid. Also, within the 66 volatile components analyzed, alcohols and acids increased, while aldehydes and ketones decreased. Lactic acid was not detected in the fermentation substrate, but an apparent increase in lactic acid content was observed along with the increased fermentation days, resulting in 2.54 ± 0.15 mg/g on day 8. Based on the tested components, the fermentation process of MMF was discriminated into three distinct stages by principal component analysis, and an optimal fermentation time of four days was proposed. The results of this study will be of great significance to clarify the characteristics of fermentation and conduce to improving quality standards of MMF.     

Fast simultaneous determination of 23 veterinary drug residues in fish,poultry, and red meat by liquid chromatography/tandem mass spectrometry

The misuses of veterinary drugs can result in the accumulation of residues in food of animal origin that can make its way to the final consumer. Herein we describe a simple method for the accurate determination of beta-lactams, quinolones, sulphonamides, and tetracyclines in fish, poultry, and red meat. No extraction cartridges were used; instead, the extraction process consisted of the addition of an organic solvents, shaking, centrifugation, and dilution. An extensive validation process demonstrated an excellent linearity (R² ≥ 0.99) for 23-drug residues. The recovery of drugs in different matrices at two concentration levels (n = 6) was in the range of 82–119%. The method was proved to be repeatable and reproducible with intra/inter-day measurements (RSDs lower than 20%). The quantification limits of drug residues were in the range of 0.8 to 45.3 ug/kg, which is well below the maximum residue limits set by most regulatory authorities. This method was successfully applied to the routine analysis of 20 fish, poultry, and red meat samples (n = 60).     

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.     

交替三线性分解算法与反相高效液相-二极管阵列检测方法相结合同时测定苯二酚的位置异构体

 利用交替三线性分解算法与反相高效液相 二极管阵列检测 (RP HPLC DAD)相结合 ,在洗脱时间为1 0 86min～ 1 399min(间隔 1 / 1 50min)、紫外吸收波长为 2 68nm～ 2 98nm(间隔 1nm)时对苯二酚位置异构体的重叠及光谱体系进行了分辨研究。分辨结果与实际结果一致。同时测定了水溶液中共存的邻苯二酚、间苯二酚和对苯二酚的含量 ,回收率分别为 (1 0 0 1± 1 0 ) % ,(99 4± 1 4) % ,(1 0 0 5± 1 7) %。研究结果表明 :该方法定量快速准确 ,实验操作步骤简单 ,解决了在干扰物存在条件下三者很难同时分辨的问题。