高效毛细管电泳分离测定水中的乙酸和氯代乙酸

用邻苯二甲酸氢钾(pH=5.4)缓冲液作为电泳的背景电解质,以十六烷基三甲基溴化铵作为电渗流抑制剂,用甲基叔丁基醚作为萃取剂处理水样,建立了一种测定水中的乙酸和氯代乙酸的简单灵敏的毛细管区带电泳(紫外检测)法.测定结果表明,分析物的迁移时间和峰面积的日内相对标准偏差分别低于0.33%和4.45%,日间相对标准偏差分别低...     

Analysis of diastereoisomer impurities in chiral pharmaceutical compounds by capillary electrophoresis

Summary Micellar electrokinetic capillary chromatography (MECC) has been applied to the separation and analysis of diastereoisomer impurities in chiral pharmaceutical compounds. Differences in separation mechanism and selectivity make MECC useful as an alternative method to HPLC for analysis of these synthetic inpurities. Advantages of MECC include high efficiency separations and low consumption of sample and solvents. Water soluble and insoluble pharmaceutical compounds are used to illustrate the separation characteristics and quantitative capabilities of this versatile new analytical technique.     

Capillary zone electrophoresis of alpha-helical diastereomeric peptide pairs with anionic ion-pairing reagents

The present study uses an unique capillary electrophoresis (CE) approach, that we have termed ion-interaction capillary zone electrophoresis (II-CZE), for the separation of diastereomeric peptide pairs where a single site in the centre of the non-polar face of an 18-residue amphipathic alpha-helical peptide is substituted by the 19 L- or D-amino acids. Through the addition of perfluorinated acids at very high concentrations (up to 400 mM), such concentration levels not having been used previously in chromatography or CE, to the background electrolyte (pH 2.0), we have been able to achieve baseline resolution of all 19 diastereomeric peptide pairs with an uncoated capillary. Since each diastereomeric peptide pair has the same sequence, identical mass-to-charge ratio and identical intrinsic hydrophobicity, such a separation by CZE has previously been considered theoretically impossible. Excellent resolution was achieved due to maximum advantage being taken of even subtle disruption of peptide structure/conformation (due to the presence of D-amino acids) of the non-polar face of the amphipathic alpha-helix and its interaction with the hydrophobic anionic ion-pairing reagents. In addition, due to the excellent resolution of diastereomeric peptide pairs by this novel CZE approach, we have also been able to separate a mixture of these closely-related alpha-helical peptides.     

毛细管电泳法分离四环素及其杂质

用毛细管电泳方法分离四环素和它的主要杂质４－差向四环素，脱水四环素，４－差向脱水四环素和２－乙酰基－２－脱酰胺四环素，相对次要的杂质氯四环素和脱甲四环素也能被分离。并系统研究了缓冲液ｐＨ，缓冲液浓度以及毛细管温度和电压对分离的影响。紫外检测波长是２７０ｎｍ，测定的相对标准偏差为１．９％。所得结果与ＨＰＬＣ方法进行了比较     

Capillary electrophoresis of signaling molecules

The emerging field of quantitative systems biology uses high-throughput bioanalytical measurements to gain a deeper understanding of biological phenomena. With the advent of instrumentation platforms, capillary electrophoresis spans a very wide range of biological applications. This short article focuses on the exploitation of capillary electrophoresis for the systems-level analysis of cell signaling molecules.     

毛细管电泳法在手性分离中的应用及进展

近年来,毛细管电泳(CE) 手性分离方法的研究主要集中在各种手性添加剂与对映体药物的匹配及实验条件的最优化选择上.目前,较为成熟的CE分离模式有:区带电泳(CZE)、凝胶电泳(CGE)、等速电泳(CITP)、胶束电动色谱(MEKC)和非水电泳(NACE)等,并已成功地用于手性化合物对映体的分离.CE手性分离研究正朝着新型手性选择剂的研制和实现与其他各种定性分析仪器及其他色谱分离模式的联用方向发展.     

毛细管电泳法分离四环素及其杂质

用毛细管电泳方法分离四环素和它的主要杂质４－差向四环素，脱水四环素，４－差向脱水四环素和２－乙酰基－２－脱酰胺四环素，相对次要的杂质氯四环素和脱甲四环素也能被分 离。     

糖类的毛细管电泳及芯片毛细管电泳

 糖类化合物在生物体内发挥多方面的作用。糖研究的复杂性在于其结构的复杂多变。高效毛细管电泳作为一种快速、高效的分离分析手段已广泛应用于糖的研究。芯片毛细管电泳是近几年来发展起来的新的分析技术 ,并已经在生命科学的研究中得到较广泛的应用。就各种糖类化合物的毛细管电泳的分析策略、检测条件及糖类化合物的芯片毛细管电泳进行了阐述 ,共 4 8篇。     

毛细管电泳在农药分析中的应用

 综述了高效毛细管电泳技术在农药分离方面的应用及发展状况 ,包括各种不同分离模式和手性选择剂的选择 ,另外还指出了该方法的优点及其发展方向。参考文献 5 0篇。     

电泳技术在纳米颗粒分离中的应用

合成纳米颗粒常在尺寸和形状方面具有广泛分布.在很多实验中,需要利用一定大小及形状的纳米颗粒的独特物理化学性质,因此,简便快速的纳米颗粒分离技术越来越受到诸多科学领域的重视.电泳技术以其高分辨率,被广泛用于多种生物大分子如核酸、蛋白质等的分离纯化.纳米颗粒在尺寸上与生物体中的蛋白复合物、细胞器和微生物等十分接近,考虑到带电纳米颗粒与生物分子在电场中的运动行为的相似性,运用电泳技术进行纳米颗粒的鉴定、分离和纯化是一种新的思路,并取得了良好的实验结果.本文主要介绍了琼脂糖凝胶电泳、毛细管电泳以及其他一些电泳技术在纳米颗粒分离中的研究进展.     

Enantiomeric Separation and Determination of R,S-Salsolinol by Capillary Electrophoresis

A new method for the quantitative determination of the enantiomers of salsolinol, an endogenous neurotoxin, was reported. Enantiomeric separation of salsolinol was obtained by capillary zone electrophoresis using hydroxypropyl-β-cyclodextrin （HP-β-CD） as chiral selector. Coupled with UV detection, this separation was applied to the determination of R,S-salsolinol in dried banana chips, and both R- and S-salsolinol were found at 40 ktg/g level.     

Capillary electrophoresis and column chromatography in biomedical chiral amino acid analysis

Free amino acids are typically quantified as the sum of their enantiomers, because in terrestrial organisms they mainly exist in the left-handed form. However, with increasing understanding of the biological significance of right-handed amino acids interest in enantioselective quantification of amino acids has steadily increased. Initially, electrophoretic and chromatographic methods using chiral (pseudo)-stationary phases or chiral eluents were applied to the separation of amino acid enantiomers. Later, derivatization of amino acids prior to chromatography with chiral reagents gained in popularity, because the diastereomers formed can be resolved on conventional reversed-phase columns. Novel multi-interaction chiral columns turned attention back to direct chiral chromatographic methods. Hyphenation to mass spectrometry has increasingly replaced optical detection because of superior selectivity, although this has not obviated the need for baseline resolution of amino acid enantiomers. Despite the progress made, enantioselective separation and quantification of amino acids remains an analytical challenge owing to frequently incomplete resolution of all naturally occurring enantiomers and insufficient sensitivity for the determination of the trace amounts of d-amino acids typically found in biological fluids and tissues. Chiral GC-MS analysis of heptafluorobutanol/pentafluoropropionanhydride amino acid derivatives on an Rt-gDEXsa column     

高效毛细管电泳拆分氯霉素前体

采用未涂层毛细管柱 (5 5cm× 5 0 μm) ,基于H3 BO3 与 β CD络合成大阴离子作为手性拆分试剂 ,在NaOH Cit溶液中加入 9 0mol/LH3 BO3 与 7 0mmol/L β CD(pH =3 0 )作为运行缓冲液 ,用高效毛细管电泳电导检测法对氯霉素前体 (PCP)进行了拆分研究。考察了影响分离的实验参数 ,同时对其拆分机理进行了初步探讨。结果表明 ,在选择的最佳实验条件下 ,氯霉素前体分子中 4个对映异构体在 2 0min内得到基线分离 ,所建立的方法分离条件简单 ,重现性好。     

毛细管电泳手性分离进展*

评述了近年来毛细管电泳手性分离的进展。以各种手性选择剂的发展为线索介绍了毛细管电泳手性分离理论、方法及应用。简要说明了分离中应注意的一些关键问题。     

手性药物的毛细管电泳拆分

以氧氟沙星、扑尔敏、特布它林和普萘洛尔为手性药物,分别采用羟丙基-β环糊精(HP--βCD)、羟丙基-β-环糊精结合羧甲基-β-环糊精(HP--βCD/CM--βCD)作手性拆分试剂,考察环糊精浓度和pH对手性选择性的影响。结果发现环糊精提供手性相互作用,而pH强烈地影响这种相互作用。以HP--βCD/CM-β-CD组成的双环糊精系统能更好地优化手性选择性,而通过调节pH可以获得需要的分离选择性、迁移次序。     

毛细管电泳在手性氨基酸拆分中的研究进展

毛细管电泳(capillary electrophoresis,CE)作为一种强有力的手性分离技术,由于操作简单、试剂消耗少及柱效高等优点,受到广泛关注,是近年来手性分离领域的研究热点.氨基酸是组成蛋白质的基本单元,且大多数氨基酸具有手性中心,手性氨基酸是生命体系的一个重要特征.具有手性中心的氨基酸,其对映体间的生物活性往往存在着较大的差异,因此,氨基酸的手性拆分对了解人体及动物生命活动起着举足轻重的作用.主要总结了近5年来毛细管电泳的3种分离模式(毛细管区带电泳、胶束电动毛细管色谱、毛细管电色谱)在氨基酸手性拆分中的发展和应用.     

Cross validation of capillary electrophoresis and high-performance liquid chromatography for cefotaxime and related impurities

Summary A micellar electrokinetic chromatography method is presented which permits separation of cefotaxime and its major related impurities. Separation was carried out at 15 kV, using 30 mM sodium dihydrogen phosphate adjusted to pH 7.2 with 5 M NaOH and which contained 165 mM sodium dodecylsulfate as electrolyte. Results obtained by capillary electrophoresis were in good agreement with those of high-performance liquid chromatography with respect to the level of the major known impurities, total impurity content and cefotaxime purity.     

Method Development of Enantiomer Separations by Affinity Capillary Electrophoresis,Cyclodextrin Electrokinetic Chromatography and Capillary Electrophoresis-Mass Spectrometry

 Capillary electrophoresis (CE) has become a powerful tool for enantiomer separations during the last decade. Since 1993, the author has investigated enantiomer separations by affinity capillary electrophoresis (affinity CE) with some proteins and by cyclodextrin electrokinetic chromatography (CDEKC) with some charged cyclodextrins (CDs). Many successful enantiomer separations are demonstrated from our study in this review article. In the enantiomer separations by affinity CE, the deterioration of detection