手性酰胺聚硅氧烷固定相的制备与气相色谱性能

以L-苯丙氨酸,L-缬氨酸为手性源,合成了二种含末端烯基,具有刚性苯基链节的新型手性酰胺单体;并通过硅氢加成方法将其接枝到含氢硅油上,制备了两种新型手性酰胺聚硅氧烷固定相.这一新方法具有简单易行,各步产率较高的优点,所制备的手性固定相具有较好的毛细管柱色谱性能.手性拆分能力和耐温性.     

Chiral separation of the four stereoisomers of a novel antianginal agent using a dual cyclodextrin system in capillary electrophoresis

Reported here is an analytical method enabling the stereochemical resolution of a new antianginal compound possessing two stereogenic centers, leading to four stereoisomers. Only one of these isomers is currently under development as a novel antianginal agent and consequently, the other three isomers are considered as unwanted chiral impurities. Therefore, an enantioselective method is required in order to check its enantiomeric purity. This paper presents a method exploiting the high efficiency of capillary electrophoresis and the complexing properties of cyclodextrins to achieve the separation of the four stereoisomers of this weakly basic compound (pKa = 7.4). For this purpose, the combination of a neutral cyclodextrin, hydroxypropyl-gamma-cyclodextrin (HP-gamma-CD), and an anionic cyclodextrin, carboxymethyl-beta-cyclodextrin (CM-beta-CD), was added to the separation buffer running in an uncoated silica capillary. After selection of the suitable cyclodextrin system, satisfactorily separation conditions were as follows: 30 mM phosphate buffer (pH 6.4) containing 10 mM of HP-gamma-CD and 10 mM of CM-beta-CD, running voltage +30 kV. The resulting run time and resolutions were respectively about 17 min and between 1.95 and 2.84. Linearity curves (0.993 < r2 < 0.998) are also shown.     

茶汤及河水中铬的形态分析

本文采用７１７型强碱性阴离子交换树脂、活性炭分离富集与偶氮胂Ⅲ光度法结合，研究了铬形态的分离及测定，提出了铬的形态分析方法，有此法测定了茶汤及河水中铬的总量，悬浮态．溶解态、无机态、有机态、Ｃｒ（Ⅲ）和Ｃｒ（Ⅵ）。茶汤中铬主要以有机态存在，而河水中铬则主要以悬浮态存在。     

环境和生物样品中铂族金属的分析研究进展

评述了近年来环境和生物样品中痕量铂族金属的分析研究进展，重点介绍了样品的预处理和分离富集技术以及检测手段等。     

Separation of structural isomers using cyclodextrin-polymers coated on silica beads

Summary Several -cyclodextrin (CD)-bonded stationary phases for high performance liquid chromatography (HPLC) were prepared, based on silica beads coated with a poly(alkylamine), [poly(ethyleneimine)(PEI)]. In order to obtain stationary phases with a high content of CD and maximum accessibility of the CD cavity, the functionalization was carried out after the coating, using the mono-tosyl derivative of CD as the intermediate. The ability of these supports to separate ortho, meta and para isomers of some disubstituted benzene derivatives was examined. The contribution of the amino groups of the polymer and of the CD cavity to the separation process is discussed. The resolution is mainly based on the difference in the stability of the complexes of the various isomers with CD. The influence of the amount of CD on the height of the theoretical plate is also studied.     

毛细管电泳无胶筛分介质分离DNA的机理

快速、高效而灵敏的分离技术对于DNA的分析是至关重要的。使用无胶筛分介质的毛细管电泳是最重要的DNA分离技术之一，通常使用无交联的高分子溶液作为无胶筛分介质。本文在介绍高分子溶液理论的基础上，综述了DNA在毛细管电泳无胶筛分介质（缠结溶液和稀溶液）中的分离机理，主要包括Ogston筛分模型、各种修正的爬行模型、瞬态缠结偶合机理及其改进机理等。     

Photo-induced Charge Separation of p-Tricyanovinyl-N,N-Dialkylanilines

In this paper,p-tricyanovinyl-N,N-dialkylanilines were synthesized as model compounds and through their spectroscopic behavior,the photo-induced electron transfer,charge separation were discussed and the aggregation in DMSO-H_2O system was investigated.     

Dynamic percolation transition induced by phase separation: A Monte Carlo analysis

The percolation transition of geometric clusters in the three-dimensional, simple cubic, nearest neighbor Ising lattice gas model is investigated in the temperature and concentration region inside the coexistence curve. We consider quenching experiments, where the system starts from an initially completely random configuration (corresponding to equilibrium at infinite temperature), letting the system evolve at the considered temperature according to the Kawasaki spinexchange dynamics. Analyzing the distributionn _l(t) of clusters of sizel at timet, we find that after a time of the order of about 100 Monte Carlo steps per site a percolation transition occurs at a concentration distinctly lower than the percolation concentration of the initial random state. This dynamic percolation transition is analyzed with finite-size scaling methods. While at zero temperature, where the system settles down at a frozen-in cluster distribution and further phase separation stops, the critical exponents associated with this percolation transition are consistent with the universality class of random percolation, the critical behavior of the transient time-dependent percolation occurring at nonzero temperature possibly belongs to a different, new universality class.     

氧氟沙星片剂和滴眼液中氧氟沙星对映体的毛细管电泳拆分及定量分析

采用环糊精及其衍生物为手性选择剂在CE上对氧氟沙星对映体进行了分离，研究了环糊精种类、浓度、分离电压、温度对分离的影响．重点考察了氧氟沙星的定量线性范围、检测限和重现性，在20-200mg／L浓度范围内，迁移时间重现性的相对标准偏差(RSD)控制在1．13％以内，峰面积重现性的RSD控制在4．3％以内，检测限为1mg／L．结果表明用20mmo1／L二甲基-β-环糊精(DM-β-CD)为手性选择剂，背景电解质为50mmo1／L Na2HPO4，pH＝3．0，不加有机添加剂情况下可得到较好的分离效果．同时，对氧氟沙星药品实样进行了分析，建主了一种市售氧氟沙星片剂和滴眼液中氧氟沙星对映体简单、快速的毛细管电泳分离、定量分析方法．     

渗透蒸发脱盐的研究

将选择性透过膜和汽化相结合的分离过程是当前的研究热点,其中采用低热导率、疏水性多孔膜的过程称膜蒸馏,而采用非多孔性半透膜的过程则称渗透蒸发。将该分离过程用于盐水脱盐已有很多报道,并已建成中试设备,但采用的大多是膜蒸馏,所用膜的成本很高。本文研究制了一种价廉并带有致密层的非对称性含钠离子聚乙烯醇(PVA)-聚乙二醇(PEG)分离膜,并用该膜对渗透蒸发脱盐进行了初步研究。 1 实验 1.1 膜制备 将一定配比的PVA与PEG及钠盐水溶液在适当温度下混溶,加入适量醛类交联剂,数分钟后在选定的基材上流涎成膜,室温下自然晾干,再经35℃～50℃控温红外线干燥。 1.2 膜结构及脱盐流程 扫描电镜拍摄的膜断面形貌图像(图1)表明,该膜为非对称膜,表层厚约13μm,其中厚约2～3/μm的上表层为疏松结构,下表层为致密结构。将该类膜用于3.5％NaCl水溶液脱盐,运行4h后再漂洗、干燥作断面Na元素波谱线分析(图2)发现,在膜下层(右侧)厚约30μm层内检测不到Na元素。脱盐流程见文献。