The use of naphthalene-2,3-dicarboxaldehyde for the analysis of primary amines using high-performance liquid chromatography and capillary electrophoresis

This paper reviews analytical methods, instrumental developments and applications for derivatization of primary amines with naphthalene-2,3-dicarboxaldehyde using fluorescence and chemiluminescence detection with capillary electrophoresis (CE) and high performance liquid chromatography (HPLC). The use of lasers as well as lamps as the excitation source for fluorescence detection is discussed. The detection limit observed with naphthalene-2,3-dicarboxaldehyde derivatization is often lower and better than those obtained with other analytical separations and other fluorescent dyes. In addition, this paper describes the crucial points that influence the stability of NDA primary amine derivatives, and summarize the separation, derivatization and migration conditions of the different techniques, with their advantages and drawbacks.     

毛细管电泳及其在朊病毒检测中的应用

本文简单介绍了毛细管电泳(CE)的发展前景,较详细地综述了毛细管电泳在朊病毒(PrPSc)检测方面的应用。CE作为1990年代末期发展最快的分析化学领域,已经在可传播性海绵状脑病(TSEs)的诊断检测方面显示了特有的优越性,成为目前唯一可以检测血中PrPSc的方法,为实现TSEs的生前诊断提供了新的思路。     

Field-amplified sample injection and in-capillary derivatization for sensitivity improvement of the electrophoretic determination of histamine

The feasibility of the combination of field-amplified sample injection (FASI) and in-capillary derivatization was explored for improving sensitivity of histamine in capillary electrophoresis (CE). Naphthalene-2,3-dicarboxaldehyde (NDA) was used as derivatization reagent. The reagent and sample was introduced by tandem mode. The derivatization was accomplished by at-inlet mode with standing time of 1.5 min. The combination of FASI and in-capillary derivatization was successfully achieved with about 400-fold concentration sensitivity enhancement compared to pre-capillary derivatization at the same set-up. The detection limit of concentration for histamine reached 1.25 x 10(-11) M by CE and fluorescence detection with S/N = 3. Parameters affecting FASI and in-capillary derivatization process including sample matrix, buffer concentration and reagent injection amount, were investigated.     

Trace level determination of substance P using capillary electrophoresis and laser-induced fluorescence

An analytical method was developed to determine the undecapetide substance P (SP) based on capillary electrophoresis (CE) with laser-induced fluorescence (LIF) detection. SP was derivatized with the fluorogenic reagent 2,3-naphthalenedicarboxaldehyde (NDA) prior to injection into the CE-LIF system. The pre-column derivatization scheme combined with injection enhancement techniques extends the detectability of SP to the subnanomolar level. Limit of detection (LOD) of 100 pM was achieved without pre-concentrating the sample prior to injection. The reproducibility for six different preparations of a standard sample containing 5 nM of SP was 6.8% RSD and that of the CE migration time was 0.08% RSD. The method was used to determine SP in a saliva sample.     

Stacking, derivatization, and separation by capillary electrophoresis of amino acids from cerebrospinal fluids

This paper describes the in-column derivatization, stacking, and separation of amino acids by CE in conjunction with light-emitting diode-induced fluorescence using naphthalene-2,3-dicarboxaldehyde (NDA). According to the relative electrophoretic mobilities and the migration direction in tetraborate solution (pH 9.3), the injection order is cyanide, then amino acids, then NDA. Once poly(ethylene oxide) (PEO) migrates through the capillary under EOF, the amino acid.NDA derivatives, amino acids, and CN- ions migrating against the EOF enter the PEO zone. As a result of increases in viscosity and possible interactions with PEO molecules, the reagents/analytes slow down such that they become stacked at the boundary. In comparison with the off-column approach to the analysis of amino acids, our proposed method provides a lower degree of interference from polymeric NDA compounds and other side products. As a result, the plot of the peak height as a function of gamma-aminobutyric acid (GABA) concentration is linear over the range from 10(-5) to 10(-8) M, with the LOD being 4 nM. We demonstrate the diagnostic potential of this approach for the determination of amino acids, including GABA and glutamine, in biological samples through the analysis of large volumes of cerebral spinal fluids without the need for sample pretreatment.     

Recent advances in capillary electrophoresis and capillary electrochromatography of pollutants

Recent advances in capillary electrophoresis (CE) and capillary electrochromatography (CEC) separation, detection and sample preparation methodologies applied for the determination of a variety of pollutants is overviewed. The reviewed literature illustrates the wide range of CE applications, indicating the continuing interest in CE and CEC in the environmental field.     

Electrophoretic separations on chips with hydrodynamically closed separation systems

This review focuses on capillary electrophoretic separations performed on capillary electrophoresis chips (CE chips) with hydrodynamically closed separation systems in a context with transport processes (electroosmotic flow (EOF)) and hydrodynamic flow (HDF)) that may accompany the separations in these devices. It also reflects some relevant works dealing with conventional CE operating under such hydrodynamic conditions. The use of zone electrophoresis (ZE), isotachophoresis (ITP) and their on-line combination (ITP-ZE) on the single-column and column-coupling CE chips with the closed separation systems and related problems are key topics of the review. Some attention is paid to sample pretreatment in the separations performed on the CE chips. Here, mainly potentialities of the ITP-ZE combination in trace analysis applications of the miniaturized systems are discussed in a broader extent. Links between the ZE separation and detection provide a frame for the discussion of current status of the detection on the CE chips. Analytical applications illustrate potentialities of the CE chips operating with the closed separation systems (suppressed HDF and EOF) to the determination of small ions present in various matrices by ZE, ITP and ITP-ZE.     

Strategies for capillary electrophoresis: Method development and validation for pharmaceutical and biological applications—Updated and completely revised edition

This review is in support of the development of selective, precise, fast, and validated capillary electrophoresis (CE) methods. It follows up a similar article from 1998, Wätzig H, Degenhardt M, Kunkel A. “Strategies for capillary electrophoresis: method development and validation for pharmaceutical and biological applications,” pointing out which fundamentals are still valid and at the same time showing the enormous achievements in the last 25 years. The structures of both reviews are widely similar, in order to facilitate their simultaneous use. Focusing on pharmaceutical and biological applications, the successful use of CE is now demonstrated by more than 600 carefully selected references. Many of those are recent reviews; therefore, a significant overview about the field is provided. There are extra sections about sample pretreatment related to CE and microchip CE, and a completely revised section about method development for protein analytes and biomolecules in general. The general strategies for method development are summed up with regard to selectivity, efficiency, precision, analysis time, limit of detection, sample pretreatment requirements, and validation.     

Determination of amino acids in tea leaves and beverages using capillary electrophoresis with light-emitting diode-induced fluorescence detection

The combination of capillary electrophoresis (CE) and light-emitting diode-induced fluorescence (LED-IF) detection has been demonstrated in the analysis of major amino acids in tea leaves and beverages. The separation efficiency of amino acids, which were derivatized with naphthalene-2,3-dicarboxaldehyde (NDA), depended on the capillary length and PEO concentration. We suggested that the interactions between the NDA derivatives and poly(ethylene oxide) (PEO) molecules are based on hydrogen bonding, hydrophobic patches, and Van der Waals forces. The magnitude of EOF and the interactions between them can be further controlled by the capillary length. The separation of 17 NDA-amino acids derivatives was completed within 16 min using 0.5% PEO and 60 cm capillary length. The relative standard deviations (R.S.D.) of their migration times (n = 5) were less than 2.7%. Additionally, the limits of detection at signal-to-noise ratio 3 for the tested amino acids ranged from 3.6 to 28.3 nM. Quantitative determination of amino acids in tea leaves and beverages was accomplished by our proposed method. This study showed that amino acid present in highest concentration in tea leaves and beverages is γ-aminobutyric acid and theanine, respectively. The experimental results suggest that our proposed methods have great potential in the investigation of the biofunction of different tea samples.     

Capillary electrophoresis/mass spectrometry relevant to pharmaceutical and biotechnological applications

Advanced analytical techniques play a crucial role in the pharmaceutical and biotechnological field. In this context, capillary electrophoresis/mass spectrometry (CE/MS) has attracted attention due to efficient and selective separation in combination with powerful detection allowing identification and detailed characterization. Method developments and applications of CE/MS have been focused on questions not easily accessible by liquid chromatography/mass spectrometry (LC/MS) as the analysis of intact proteins, carbohydrates, and various small molecules, including peptides. Here, recent approaches and applications of CE/MS relevant to (bio)pharmaceuticals are reviewed and discussed to show actual developments and future prospects. Based on other reviews on related subjects covering large parts of previous works, the paper is focused on general ideas and contributions of the last 2 years; for the analysis of glycans, the period is extended back to 2006.     

2020年毛细管电泳技术年度回顾

该文为2020年毛细管电泳(capillary electrophoresis,CE)技术年度回顾.归纳总结了以"capillary electro-phoresis-mass spectrometry"或"capillary isoelectric focusing"或"micellar electrokinetic...     

Capillary electrophoresis of inorganic anions

This review deals with the separation mechanisms applied to the separation of inorganic anions by capillary electrophoresis (CE) techniques. It covers various CE techniques that are suitable for the separation and/or determination of inorganic anions in various matrices, including capillary zone electrophoresis, micellar electrokinetic chromatography, electrochromatography and capillary isotachophoresis. Detection and sample preparation techniques used in CE separations are also reviewed. An extensive part of this review deals with applications of CE techniques in various fields (environmental, food and plant materials, biological and biomedical, technical materials and industrial processes). Attention is paid to speciations of anions of arsenic, selenium, chromium, phosphorus, sulfur and halogen elements by CE.     

CE determination of small ions: methods and techniques

This paper provides an overview on the current status of capillary electrophoresis (CE) in the analysis of inorganic and charged small organic species. The various CE strategies used to improve the separation of ionic analytes are summarized. Technical developments in the design of improved detection systems are described. A brief account of their advantages and limitations is given. The potential use of these devices for miniaturized CE systems is also described. Finally, special attention is focused on the on-capillary preconcentration techniques developed in attempts to overcome the poor detectability of CE. Recent review articles are frequently cited to provide readers with a source of information about pioneering work, theoretical treatments, and specific applications.     

HPLC-fluorescence detection and MEKC-LIF detection for the study of amino acids and catecholamines labelled with naphthalene-2,3-dicarboxyaldehyde

Naphthalene-2,3-dicarboxyaldehyde (NDA) is commonly used for detection of primary amines in conjunction with their separation with HPLC and CE. The fluorescence of the derivatives can be measured by a conventional fluorometer or via LIF. NDA is a reactive dye, which can replace o-phthaldehyde (OPA) and provides for derivatives which are considerably more stable than OPA derivatives. In addition, NDA can be used to derivatize primary amines at concentrations as low as 100 pM. In this work, HPLC/fluorescence and MEKC/LIF experiments were performed to separate/detect six neuroactive compounds, the amino acids, Gly, Glu, Asp, gamma-aminobutyric acid (GABA) and the catecholamines, dopamine and noradrenaline. The two methods were compared in terms of performance of separation. The amino acids can be separated in HPLC in less than 30 min and an identical separation is obtained in CE using MEKC and lithium salts with greater resolution (the number of theoretical plates was approximately 5000 for HPLC and 200 000 for MEKC). The lowest detected concentration was in the range of 0.1 nM for CE/LIF. The presence of a high salt concentration does not affect the separation of the samples. Examples of the analysis of microdialysate samples as well as amino acids in Ringer's solution are presented.     

Electrophoretically mediated microanalysis

This review describes the existing developments in the use of the capillary electrophoretic microanalytical technique for the in-line study of enzyme reaction, electrophoretically mediated microanalysis (EMMA). The article is divided into a number of parts. After an introduction, the different modes, basic principle, procedure, and some mathematical treatments of EMMA methodology are discussed and illustrated. The applications of EMMA for enzyme assay and for non-enzymatic determination are summarized into two tables. In addition to classical capillary electrophoresis (CE) instrument EMMA, special emphasis is given to a relatively new technique: EMMA on CE microchip. Finally, conclusions are drawn.     

A decade of capillary electrophoresis

Since the introduction of the first commercial capillary electrophoresis (CE) instrument a decade ago, CE applications have become widespread. Today, CE is a versatile analytical technique which is successfully used for the separation of small ions, neutral molecules, and large biomolecules and for the study of physicochemical parameters. It is being utilized in widely different fields, such as analytical chemistry, forensic chemistry, clinical chemistry, organic chemistry, natural products, pharmaceutical industry, chiral separations, molecular biology, and others. It is not only used as a separation technique but to answer physicochemical questions. In this review, we will discuss different modes of CE such as capillary zone electrophoresis, micellar electrokinetic chromatography, capillary gel electrophoresis, capillary isoelectric focusing, and capillary electrochromatography, and will comment on the future direction of CE, including array capillary electrophoresis and array microchip separations.     

A gravity-independent single-phase electrode reservoir for capillary electrophoresis applications

Capillary electrophoresis (CE) holds great promise as an in situ analytical technique for a variety of applications. However, typical instrumentation operates with open reservoirs (e.g., vials) to accommodate reagents and samples, which is problematic for automated instruments designed for space or underwater applications that may be operated in various orientations. Microgravity conditions add an additional challenge due to the unpredictable position of the headspace (air layer above the liquid) in any two-phase reservoir. One potential solution for these applications is to use a headspace-free, flow-through reservoir design that is sealed and connected to the necessary reagents and samples. Here, we demonstrate a flow-through high-voltage (HV) reservoir for CE that is compatible with automated in situ exploration needs, and which can be electrically isolated from its source fluidics (in order to prevent unwanted leakage current). We also demonstrate how the overall system can be rationally designed based on the operational parameters for CE to prevent electrolysis products generated at the electrode from entering the capillary and interfering with the CE separation. A reservoir was demonstrated with a 19 mm long, 1.8 mm inner diameter channel connecting the separation capillary and the HV electrode. Tests of these reservoirs integrated into a CE system show reproducible CE system operation with a variety of background electrolytes at voltages up to 25 kV. Rotation of the reservoirs, and the system, showed that their performance was independent of the direction of the gravity vector.     

Analysis of drugs, natural and bioactive compounds containing phenolic groups by capillary electrophoresis coupled to mass spectrometry

This review summarizes the use of capillary electrophoresis (CE) coupled to mass spectrometry (MS) for the analysis of phenolic compounds and its latest developments. Special attention is paid to the different interfaces. The instrumental setups are discussed and demonstrated in a high number of real applications.     

毛细管电泳安培检测技术进展

对毛细管电泳离柱和柱端安培检测方式、不同形式电极在安培检测中的应用、安培检测在芯片毛细管电泳中的应用、安培检测池等内容进行了总结和讨论 ,并预测了安培检测技术未来发展方向     

Optimal configuration of capillary electrophoresis microchip with expansion chamber in separation channel

This study develops a novel capillary electrophoresis (CE) microfluidic device featuring a conventional cross-form injection system and an expansion chamber located at the inlet of the separation channel. The combined injection system/expansion chamber arrangement is designed to deliver a high-quality sample band into the separation channel such that the detection performance of the device is enhanced. Numerical simulations are performed to investigate the electrokinetic transport processes in the microfluidic device and to establish the optimal configuration of the expansion chamber. The results indicate that an expansion chamber with an expansion ratio of 2.5 and an expansion length of 500 microm delivers a sample plug with the correct shape and orientation. With this particular configuration, the peak intensities of the sample are sharp and clearly distinguishable in the detection region of the separation channel. Therefore, this configuration is well suited for capillary electrophoresis applications which require a highly sensitive resolution of the sample plug. The novel CE microfluidic device developed in this study has an exciting potential for use in high-performance, high-throughput chemical analysis applications and in many other applications throughout the field of micro-total-analysis-systems.