毛细管电泳在火炸药研究中的应用

近年来,毛细管电泳以其高效、快速、微量的特点,在火炸药分析领域被广泛应用并迅速发展。本文从毛细管区带电泳、胶束电动毛细管色谱、毛细管电色谱、芯片毛细管电泳、微乳毛细管电动色谱这五种毛细管电泳的模式出发,结合本实验室的最新研究进展,综述毛细管电泳在火炸药研究中的应用。     

毛细管电泳涂层柱技术的进展

毛细管电泳涂层柱是解决蛋白质在毛细管壁吸附的最有效的方法。较为系统地综述了毛细管电泳涂层柱的几种制作方法,指出了毛细管电泳涂层柱（包括毛细管电色谱柱）的发展趋势,３９篇。     

毛细管电泳免疫分析

本文首先对毛细管电泳免疫分析进行了对比。然后,从毛细管电泳免疫分析的不同免疫模式和不同电泳模式两方面以及技术进展,对近几年毛细管电泳免疫分析的多个应用领域进行了综述。     

毛细管电泳中的毛细管区段灌注及其相关技术

毛细管区段灌注是一种随手性毛细管电泳、亲和毛细管电泳和胶束电动力色谱-质谱发展而产生的实验技术。由于它能消除采用以上方法时遇到的缓冲溶液对检测的影响。因此引起人们的关注。本文对区段灌注技术的原理,区段灌注技术在手性毛细管电泳、亲和毛细管电泳和胶束电动力色谱中的应用,以及目前区段灌注技术存在的一些问题进行了评述。本文还对由区段灌注技术发展而来的逆流毛细管电泳、液相预柱毛细管电泳、多步配体进样等实验技术进行了简介。     

毛细管电泳的原理及应用第一讲毛细管电泳简介

毛细管电泳的原理及应用第一讲毛细管电泳简介     

毛细管电泳指纹图谱及毛细管电泳-质谱联用在中药质量控制中的作用

以作者多年从事毛细管电泳、毛细管电泳-质谱联用及其指纹图谱对中药的研究成果为基础,介绍了毛细管电泳实验条件的优化方法、毛细管电泳指纹图谱的研究方法与评价方法及其在中药质量控制中的作用。     

α-干扰素的液相色谱/毛细管电泳两维分离分析

用亲和色谱/反相色谱、亲和色谱/毛细管电泳和凝胶色谱/毛细管电泳等两维系统, 对白细胞提取液中的α-干扰素进行分离分析, 并对结果进行比较,充分肯定了亲和色谱/毛细管电泳联用在蛋白质类药物制备纯化中的显著作用,以及毛细管电泳作为此类药物分析工具的可能性。     

集成毛细管电泳芯片及其制作技术的进展

集成毛细管电泳芯片是一个新兴的微量分析装置,它具有高效、快速、度样用量少、节约药品等优点。文章回顾了集成毛细管电泳芯片的历史,介绍了毛细管电泳芯片在原材料、制作方法、表征、进样、分离、检测等方面的进展,并展望了毛细管电泳芯片的前景。     

流动注射-毛细管电泳联用及应用进展

流动注射是一种高效进样及在线溶液处理手段。毛细管电泳是一种高分离效率、高选择性的分析技术,但传统的毛细管电泳间歇式进样方式效率低且难用于过程分析,将流动注射进样技术与毛细管电泳结合,既弥补了毛细管电泳的进样缺陷,又可兼具两者的优点。有关两种技术的联用一直都在探索之中。文中对近年流动注射一毛细管电泳联用及应用研究进行了综述。     

非水溶液毛细管电泳

评述了非水溶液毛细管电泳的应用及发展，对非水溶液毛细管电泳的原理及应用情况作了简要叙述，有机试剂在毛细管电泳中的加入，扩大了分析物质的范围，以纯有机试剂作电泳介质，具有许多水溶液毛细管电不能比拟的优点。     

Practical aspects of using methacrylate-ester-based monolithic columns in capillary electrochromatography

Methacrylate-ester-based monoliths containing quaternary ammonium groups were prepared in situ in capillary columns and in simultaneous experiments in vials, employing thermal initiation. The chromatographic properties of the monoliths were determined with capillary electrochromatography (CEC), and their morphology was studied with mercury-intrusion porosimetry on the bulk materials. Materials with different, well repeatable pore-size distributions could be prepared. A satisfactory column-to-column and run-to-run repeatability was obtained for the electro-osmotic mobility, the retention characteristics (k-values) and the efficiency on the columns prepared and tested in the CEC mode. A relatively high electro-osmotic flow was observed in the direction of the positive electrode. The electro-osmotic mobility was found to be influenced only marginally by mobile-phase parameters such as the pH, ionic strength, and acetonitrile content. The retention behavior of the monolithic columns was similar to that of columns packed with C18-modified silica particles. Columns could be prepared with optimum plate heights ranging from 6 microm for unretained compounds to 20 microm for well retained (k=2.5) polyaromatic hydrocarbons. However, for specific analytes a - still unexplained - lower chromatographic column efficiency was observed.     

一种新型超支化聚酯物理吸附涂层毛细管电泳柱的制备及其对碱性蛋白质的分离

采用一步法和准一步法合成了以季戊四醇为核的两个系列的超支化聚酯,利用红外光谱、羟值测定等手段对分子结构进行了表征。利用超支化聚合物低粘度的特点,用物理吸附方法将其涂于毛细管电泳柱内壁,使其在毛细管内壁上形成稳定的超支化聚酯涂层。该涂层在pH 3.0~7.0范围内能够有效地抑制电渗流和蛋白质在毛细管壁上的吸附,在pH 5.0的缓冲液中分离碱性蛋白质时,分离柱效可达105塔板/m,具有良好的分离效果。     

Polyethyleneimine-bonded phases in the separation of proteins by capillary electrophoresis

A hydrophilic, positively charged, durable coating has been developed for capillary electrophoresis of macromolecules. Polyethyleneimine is adsorbed to the inner wall of fused silica capillaries and the adsorbed coating cross-linked into a stable layer. Capillaries of polyethyleneimine-coated silica gave unique separations owing to the reversal of electro-osmotic flow caused by the positively charged coating. The resulting coating was stable from pH 2-12 and could be used over a wide pH range without substantial change in electro-osmotic flow. High-molecular-weight polymers were needed to give thick coatings which mask silanol groups on the wall. Proteins were resolved quickly and efficiently with good recovery using capillaries of 50 cm in length.     

Non-aqueous capillary electrophoretic separation of enantiomeric amines with (-)-2,3:4,6-di-O-isopropylidene-2-keto-L-gulonic acid as chiral counter ion

(-)-2,3:4,6-Di-O-isopropylidene-2-keto-L-gulonic acid [(-)-DIKGA] has been introduced as a chiral counter ion in non-aqueous capillary electrophoresis. High enantioresolutions (R(s)> or =3) were obtained for amines, e.g., pronethalol, labetalol and bambuterol. Methanol containing NaOH and (-)-DIKGA was used as the background electrolyte. The counter ion concentration and the nature of the injection medium were found to affect the chiral separation. Covalent coating of the fused-silica capillary reduced the electro-osmotic flow resulting in improved enantioresolutions.     

Determination of global DNA methylation level by capillary electrophoresis using octyl-modified quaternized cellulose as an electrolyte additive

A new cellulose derivative, octyl-modified quaternized cellulose (OMQC), was synthesized and used as electrolyte additive for the analysis of 5-methylcytosine by capillary electrophoresis with UV detection. While added in the background electrolyte, OMQC carrying octyl groups and quaternary ammonium groups exhibited dynamic coating ability. Capillary coated with OMQC was able to generate a stable anodal electro-osmotic flow even at pH 12.0. After several running conditions were optimized, a new method for quantification of genomic methylation level was developed on the basis of hydrolysis of DNA by formic acid and separation of nucleic acid bases by capillary electrophoresis. Cytosine and 5-methylcytosine were separated with a resolution near 4.0 in less than 10 min. The detection limits (S/N?=?3) were 1.1 and 1.5 μg/mL for cytosine and 5-methylcytosine, respectively.     

Capillary electrochromatography with 1.5 μm ODS-modified non-porous silica spheres

Summary The particle realization of electrochromatography on capillaries packed with 1.5 μm ODS-modified non-porous silica spheres is demonstrated. In order to realize stable separation conditions it is crucial to add sodium dodecylsulphate (SDS) to the mobile phase and to pressurize both buffer vials at 10 bar. The presence of SDS stabilizes the current and makes the electro-osmotic flow in the packing more uniform so that no air bubbles are generated at high field strengths. The capillary columns are extremely efficient and on a 24 cm long column about 120,000 plates can be generated (a reduced plate height of about 1.3). The columns are very stable and no loss in efficiency was found after using a column continuously for two months.     

A new method of evaluating the average electro-osmotic velocity in microchannels

A new and simple method to evaluate the average electro-osmotic flow velocity in microchannels is presented in this paper. In this method, the average electro-osmotic flow velocity is determined by using the slope of the measured current-time relationship during the electro-osmotic flow of one solution replacing another similar solution. The two solutions have the same electrolyte and a small difference in ionic concentration. Careful experiments were conducted to measure the electrical current change with time during such a displacing process under a constant applied electrical field. KCl and LaCl3 electrolyte solutions and 10-cm-long polyamide-coated silica capillary tubes of 100 and 200 microm in internal diameter were used in this study. The average velocities were determined by using the slope method. A numerical model was also developed to predict the average velocity of such an electro-osmotic flow. An excellent agreement in the average velocities between the slope method and the model predictions was found.     

矩形截面毛细管电泳和二维分离

在石英单晶表面制成矩矩截面毛细管柱中进行电泳实验。由于矩形柱比圆形柱有更大散热侧面积且石英单晶的导热性能远无于熔融石英，所以可施加较高的场强，不仅提高了柱效，而且缩矩了分离时间。两相交的通道之间形成自然连接，可实现二维分离，并消除死体积。     

Sample introduction and separation in capillary electrophoresis, and combination with mass spectrometric detection

Capillary-electrophoresis methods are attracting interest owing to the ability to yield rapid high-resolution separations, but many aspects, such as sample injection, separation conditions and detection, need further development. Effects related to sample injection and buffer composition have been investigated. Automated methods for electromigration injection of nl-size sample volumes are shown to give a precision of approximately +/-1%. Problems encountered with manual injection procedures have been examined by an electric field reversal technique. The effect of buffer pH on capillary zone-electrophoresis (CZE) separations can be attributed to changes in electro-osmotic flow velocities and to changes in the isoelectric points of analytes. The interfacing of capillary electrophoresis with mass spectrometry is described and demonstrated for a range of conditions, with a quaternary phosphonium salt mixture. Separations obtained by CZE and capillary isotachophoresis are compared and the relative advantages of the two techniques discussed.     

Separation of Hydroxybenzoic Acid Isomers by Capillary Zone Electrophoresis

Abstract

Capillary zone electrophoresis is a highly efficient analytical technique that has been shown to be particularly useful for the analysis of isomers. Using a cathodic injection and anodic detection scheme, ortho-, meta- and para-hydroxybenzoic acids were separated in a fused-silica capillary column with a phosphate buffer at pH 10.3 (25.0 mmol/1 phosphate + 0.20 mmol/1 cetyltrimethylammonium bromide (CTAB) + 10% (v/v) 1-propanol with an applied voltage of 10 KV followed by direct UV detection. The use of CTAB as electroosmotic flow modifier allows the rapid separation of the three isomers by reversing the direction of electro-osmotic flow. The influence of pH, CTAB concentration and organic solvents on the migration behaviour of the solutes were also studied.