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131.
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. 相似文献
132.
133.
建立了高效毛细管电泳结合柱上紫外检测测定单胺类神经递质多巴胺(dopamine,DA)和5_羟色胺(5_hydroxytryptamine,5_HT)的毛细管电泳方法 ,优化了缓冲液 pH值、浓度、电压等实验参数 ;结果表明 ,在优化的实验条件下 ,多巴胺、3,4_二羟苄胺 (3,4_dihydroxybenzylamine)和5_羟色胺在10min内得到很好的分离 ,检出限分别为2.02×10 -5mol/L,1.01×10 -5mol/L,1.20×10 -5mol/L ;该法简便、快速 ,样品用量少 ,结果准确 ,重现性好 相似文献
134.
非水介质毛细管电泳电导检测舒血宁片中槲皮素含量 总被引:6,自引:0,他引:6
以甲醇:水=70:30的体系为分离介质,柠檬酸-三(羟甲基)氨基甲烷(Citric acid-Tris)为支持电解质,使用电导检测,对槲皮素及其制剂舒血宁片进行了毛细管电泳分离检测,对电泳介质的种类、浓度、表观pH值以及操作电压和进样时间对分离的影响进行了研讨,并对分离检测机理进行了探讨。建立的测定槲皮素的方法的线性范围为:8.0-160.0mg/L;峰面积的RSD(n=6)为1.7%,检出限为1.0mg/L;样品加标回收率为92.8%-98.2%。 相似文献
135.
A method for preparation of capillary columns and traps with a very thick film (up to 100 μm) of stationary phase is described. The principle of this method is based on an immediate fixation of a film of prepolymer, formed during dynamic coating. Thus, the development of film irregularities, such as are caused by Rayleigh instability is avoided. Fixation of the film is conveniently accomplished by heat-accelerated crosslinking as was demonstrated in this work, where a commercially available silicone prepolymer (Sylgard 184, Dow Corning) was employed. The low phase ratio columns which thus can be prepared are interesting both in chromatography with dense mobile phases and as enrichment devices. Examples of the latter application are shown, where trace organic components from air and water were concentrated. 相似文献
136.
本文叙述氨基酸及其对映体的全氟酰基烷基脂(O-异丙基、-异丁基、-正丁基;N(O,S)-三氟乙酰基,TFA、-七氟丁酰基,HFB)在Chirasil-Val上的洗脱特性。随烷基取代增大,保留时间增加;用HFB代替TFA,对映体的分离因子降低。此外,DL-氨基酸与另丁醇衍生,生成的对映及非对映衍生物在Chirasil-Val上可拆分成四个色谱峰。 相似文献
137.
Muhammad Ilyas Sarwar Sonia Zulfiqar Zahoor Ahmad 《Colloid and polymer science》2007,285(15):1733-1739
Fluoro-aramid-based sol/gel-derived nanocomposites were synthesized by condensing a mixture of 4,4′-(hexafluoro-isopropylidene)dianiline
and 1,3-phenylenediamine with terephthaloylchloride (TPC) in dimethylacetamide. TPC was added in slight excess to produce
amide chains with carbonyl chloride end groups and then replaced with alkoxy groups using aminophenyltrimethoxysilane to develop
bonding with the silica network. Mechanical, dynamic mechanical thermal, water absorption and morphological measurements were
carried out on the thin hybrid films. Increase in the tensile strength and modulus was observed as compared to pristine polyamide.
The thermal decomposition temperature was found in the range of 400–500 °C. The water absorption was found to be reduced with
higher silica content. The glass transition temperature and the storage moduli increased with increasing silica concentration.
The maximum increase in the T
g value (345 °C) was observed with 20 wt% silica. Scanning electron microscopy revealed the uniform distribution of silica
in the matrix with an average particle size ranging from 8 to 50 nm. 相似文献
138.
139.
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。 相似文献
140.
Summary The chromatographic performance of newly developed dicyanobiphenyl polysiloxane stationary phases were evaluated and compared
with the performance of other polar stationary phases, including the previously reported monocyanobiphenyl polysiloxanes.
Due to the unique combination of polarizable biphenyl and polar cyano functionalities in the side chains of the flexible polysiloxane
backbone, and by virtue of their mild liquid crystalline properties, the new stationary phases provide excellent resolution
of a wide variety of analytes, both polar and nonpolar, in both GC and SFC. They can be easily coated and cross-linked in
open tubular columns, and the resultant columns demonstrate excellent efficiency and performance at temperatures up to 280–300°C.
The new stationary phases exhibit enhanced selectivities for various types of isomeric compounds. 相似文献