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Preconcentration
Kinds of Preconcentration Terms modified by Preconcentration Selected AbstractsPreconcentration and matrix elimination for the determination of Pb(II), Cd(II), Ni(II), and Co(II)by 8-hydroxyquinoline anchored poly(styrene-divinylbenzene) microbeadsJOURNAL OF APPLIED POLYMER SCIENCE, Issue 4 2008Hakan A Abstract Poly(styrene-divinylbenzene), PS-DVB, microbeads were modified with 8-hydroxyquinoline (8-HQ) following nitration, reduction of NO2 to NH2, and conversion of NH2 to diazonium salt. Characterization of pristine, NO2, NH2, NN+Cl,, and 8-QH functional groups modified microbeads was made by Fourier transform-infrared spectrometry (FTIR) and porosimetry. Total reflectron-X-ray florescence spectrometer (TXRF) was used to test the affinity of the 8-HQ modified microbeads to toxic metal ions. 8-HQ-modified microbeads were used to examine the adsorption capacity, recovery, preconcentration, and the matrix elimination efficiency for Pb(II), Cd(II), Ni(II), and Co(II) ions as a function of changing pH, initial metal-ion concentrations, and also equilibrium adsorption time of the studied metal ions. Preconcentration factors for the studied toxic metal ions were found to be more than 500-fold and recovery between 93.8% and 100.6%. Ultratrace toxic metal-ion concentrations in sea water were determined easily by using modified microbeads. Reference sea-water sample was used for the validation of the method, and it was found that recovery, preconcentration, and the matrix elimination were performed perfectly. For the desorption of the toxic metal ions, 3M of HNO3 was used and desorption ratio shown to be more than 96%. © 2007 Wiley Periodicals, Inc. J Appl Polym Sci, 2008 [source] Preconcentration and Determination of Copper(II) Using Octadecyl Silica Membrane Disks Modified by 1,5-Diphenylcarhazide and Flame Atomic Absorption SpectrometryCHINESE JOURNAL OF CHEMISTRY, Issue 11 2007Ali MOGHIMI Abstract A simple and reproducible method for the rapid extraction and determination of trace amounts of copper(II) ions using octadecyl-bonded silica membrane disks modified by 1,5-diphenylcarbazide (DPC) and atomic absorption spectrometry was presented, which was based on complex formation on the surface of the ENVI-18 DISKTM disks followed by stripping of the retained species by minimum amounts of appropriate organic solvents. The elution was efficient and quantitative. The effect of potential interfering ions, pH, ligand amount, stripping solvent, and sample flow rate were also investigated. Under the optimal experimental conditions, the break-through volume was found to be about 1000 mL providing a preconcentration factor of 400. The maximum capacity of the disks was found to be (255±5) µg for Cu2+, and the limit of detection of the proposed method was 5 ng per 1000 mL. The method was applied to the extraction and recovery of copper in different water samples. [source] Study on Preconcentration of Trace Copper Using Microcrystalline Triphenylmethane Loaded with Malachite GreenCHINESE JOURNAL OF CHEMISTRY, Issue 4 2007Yong Liang Abstract The paper describes a novel method for copper preconcentration using microcrystalline triphenylmethane loaded with malachite green prior to the determination by the flame atomic absorption spectrometry (FAAS). Under the optimum conditions, Cu(II) can be totally adsorbed on the surface of microcrystalline triphenylmethane, and completely separated from Pb(II), Cd(II), Co(II), Cr(III), Ni(II), Mn(II), Fe(III) and Al(III) by controlling acidity. The preconcentration factor of this proposed method is 200. The recovery is in a range of 97.5%,105%. The relative standard deviation (RSD) is not beyond 3.0%. The proposed method has been successfully applied to the determination of trace copper in various water samples with satisfactory results. [source] Stripping Voltammetry at Microdisk Electrode Arrays: TheoryELECTROANALYSIS, Issue 24 2009Abstract Anodic stripping voltammetry (ASV) is an extremely powerful tool for detection of metal ions in solution through a two step process of preconcentration of the metal at the electrode surface, followed by electrodissolution. The second phase produces an electroanalytical response proportional to the amount of material deposited in the first phase. This paper utilizes theory to explore the electrochemical signals produced when considering ASV at a microelectrode or ultramicroelectrode arrays. The theory outlined is applicable mostly to thin mercury film absorption and metal adsorption. [source] Calixarene/Nafion-Modified Bismuth-Film Electrodes for Adsorptive Stripping Voltammetric Determination of LeadELECTROANALYSIS, Issue 17-18 2009Ferenc Torma Abstract This paper presents an enhanced adsorptive stripping voltammetric procedure (AdSV) for the determination of Pb2+, which relies on the accumulation of the metals at a calixarene-based chemically modified bismuth-film electrode on glassy carbon substrate. Following the accumulation of the target metals at open circuit and a medium exchange, both the square wave anodic stripping detection of the metal ions and the in situ bismuth-film formation was performed simultaneously in a Bi3+ containing supporting electrolyte. The analysis of Pb2+ under optimized conditions resulted in stripping responses with good linearity (in the range 0.05,0.6,,M) and precision (RSD=1.12% at 0.2,,M Pb2+; n=10) and low detection limit (0.02,,g/L at 10,min preconcentration). The determination of Pb2+ (0.4,,M) at 100-fold excess of interfering ions (Cd2+, Cu2+ and Zn2+) yielded well resolved lead signal. The analytical utility of the method elaborated was tested in the analysis of trace Pb2+ in environmental water samples. [source] Voltammetric Detection of Lead(II) Using Amide-Cyclam- Functionalized Silica-Modified Carbon Paste ElectrodesELECTROANALYSIS, Issue 15 2009Stéphanie Goubert-Renaudin Abstract 2-(4,8,11-Triscarbamoylmethyl-1,4,8,11-tetraazacyclotetradec-1-yl)acetamide (TETAM) derivatives bearing 1, 2, or 4 silylated arms have been synthesized and grafted to the surface of silica gel and ordered mesoporous silica samples. The resulting organic-inorganic hybrids have been incorporated into carbon paste electrodes and applied to the preconcentration electroanalysis of Pb(II). The attractive recognition properties of these cyclam derivatives functionalized with amide pendent groups toward Pb(II) species and the highly porous structure of the adsorbents can be exploited for the selective and sensitive detection of the target analyte. Various parameters affecting the preconcentration and detection steps have been discussed with respect to the composition and pH of both accumulation and detection media, the nature of the adsorbent (number of silylated groups linking the macrocycle to silica, texture of materials), the accumulation time, and the presence of interfering cations. Under optimal conditions and for 2,min accumulation at open-circuit, the voltammetric response increased linearly with the Pb(II) concentration in a range extending from 2×10,7 to 10,5,M, while a longer accumulation time of 15,min afforded a linear calibration curve between 10,8 and 10,7,M with a detection limit of 2.7×10,9,M which is well below the European regulatory limit of lead in consumption water. [source] Quantitative Analysis of Prometrine Herbicide by Liquid,Liquid Extraction Procedures Coupled to Electrochemical MeasurementsELECTROANALYSIS, Issue 6 2009V. Juarez Abstract A sensitive method is proposed for the preconcentration and quantification of the herbicide Prometrine (PROM) at a liquid-liquid interface employing square-wave voltammetry. The preconcentration stage was based on liquid-liquid extraction methodology and the PROM quantification was carried out from the peak current of square-wave voltammograms. Under the experimental conditions employed, linear calibration curves in the concentration range 1.0×10,6,M,5.0×10,5,M, with detection limit equal to 1.5×10,6,M were obtained without pretreatment of the samples. This linear range, as well as detection limit could be extended towards lower concentrations when a pretreatment procedure was employed. In this way, linearity of calibration curves between 8.0×10,8,M and 2.4×10,7,M and detection limit of 1.0×10,7,M, were observed. On the other hand, the standard addition method was also used as an alternative and an appropriated quantification technique for this system. A linear concentration range between 1.0×10,6,M and 2.7×10,5,M, with a correlation coefficient of 0.997, was obtained. This procedure has also a promising application in the separation of herbicides from other interferents, present in real samples, previous to their quantification. [source] Current-Free Deposition of Prussian Blue with Organic Polymers: Towards Improved Stability and Mass Production of the Advanced Hydrogen Peroxide TransducerELECTROANALYSIS, Issue 3-5 2009Anastasiya Abstract We report on a novel approach for open-circuit (current-free) deposition of Prussian blue. Synthesis of Prussian blue is carried out by reduction of ferric ferricyanide with organic molecules, which are known to form polymers upon oxidation. The proposed interfacial deposition is a result of the synthesis in the presence of electrode support due to preconcentration of precursors at the interface. The resulting modified electrodes displayed the dramatically improved operational stability in hydrogen peroxide continuous monitoring with no loss of either electrochemical or analytical performance characteristics compared to electrodes with electrochemically deposited Prussian blue. The shown possibility to deposit stable films with regular structure in the absence of any external voltage could open new horizons for sensor science. [source] Determination of Trace Amounts of Copper in Tap Water Samples with a Calix[4]arene Modified Carbon Paste Electrode by Differential Pulse Anodic Stripping VoltammetryELECTROANALYSIS, Issue 10 2007Çelik Canpolat Abstract A calix[4]arene modified carbon paste electrode was used for trace determination of copper. The study of the preconcentration of copper as well as the other heavy metal ions at the modified electrode, with subsequent measurement by differential pulse anodic stripping voltammetry (DPASV), indicates the efficient open-circuit accumulation of the analytes onto the electrode. Many parameters such as the composition of the paste, pH, preconcentration time and stirring rate influence the response of the measurement. The procedure was optimized for copper determination. For a 10-minute preconcentration time at pH,6.5,7.5, the detection limit (LOD) was 1.1,,g L,1. The optimized method was successfully applied to the determination of copper in tap water sample by means of standard addition procedure. The copper content of the sample was comparable with the result obtained with AAS method. [source] Simultaneous Determination of Quinoline and Pyridine Compounds in Gasoline and Diesel by Differential Pulse VoltammetryELECTROANALYSIS, Issue 6 2007Leonardo Abstract The presence of trace basic organonitrogen compounds such as quinoline and pyridine in derivative petroleum fuels plays an important role in maintaining the engines of vehicles. However, these substances can contaminate the environment and so must be controlled because most of them are potentially carcinogenic and mutagenic. For these reasons, a reliable and sensitive method was developed for the determination of basic nitrogen compounds in fuel samples such as gasoline and diesel. This method utilizes preconcentration on an ion,exchange resin (Amberlyte IR,120,H) followed by differential pulse voltammetry (DPV) on a glassy carbon electrode. The electrochemical behavior of quinoline and pyridine as studied by cyclic voltammetry (CV) suggests that their reduction occurs via a reversible electron transfer followed by an irreversible chemical reaction. Very well resolved diffusion-controlled voltammetric peaks were obtained in dimethylformamide (DMF) with tetrabutylammonium tetrafluoroborate (TBAF4 0.1,mol L,1) for quinoline (,1.95,V) and pyridine (,2.52,V) vs. Ag|AgCl|KClsat reference electrode. The proposed DPV method displayed a good linear response from 0.10 to 300,mg L,1 and a limit of detection (LOD) of 5.05 and 0.25,,g L,1 for quinoline and pyridine, respectively. Using the method of standard additions, the simultaneous determination of quinoline and pyridine in gasoline samples yielded 25.0±0.3 and 33.0±0.7,mg L,1 and in diesel samples yielded 80.3±0.2 and 131±0.4,mg L,1, respectively. Spike recoveries were 94.4±0.3% and 101±0.5% for quinoline and pyridine, respectively, in the fuel determinations. This proposed method was also compared with UV-vis spectrophotometric measurements. Results obtained for the two methods agreed well based on F and t student's tests. [source] Catalytic Adsorptive Stripping Voltammetric Procedure for Determination of Total Chromium in Environmental MaterialsELECTROANALYSIS, Issue 12 2006gorzata Grabarczyk Abstract A sensitive catalytic adsorptive stripping voltammetric procedure for determination of traces of total chromium in environmental samples is reported. The method is based on the preconcentration of a Cr(III)H2DTPA complex by adsorption at the HMDE from an acetate buffer solution at the potential ,1.0,V vs. Ag/AgCl. Total chromium was determined as Cr(III) after reduction of Cr(VI) to Cr(III) by NaHSO3. In order to stabilize the signal of Cr(III) the measurements were performed at 5,°C. The calibration graph for chromium for an accumulation time of 60,s was linear in the range from 5×10,10 to 5×10,8,mol L,1. The relative standard deviation for a chromium concentration of 1×10,8,mol L,1 was 3.9% (n=5). The detection limit for accumulation time of 60,s was about 8×10,11,mol L,1. The validation of the procedure was performed by the analysis of the certified reference materials. [source] Electrochemically-Induced Deposition of Amine-Functionalized Silica Films on Gold Electrodes and Application to Cu(II) Detection in (Hydro)Alcoholic MediumELECTROANALYSIS, Issue 19 2005Alain Walcarius Abstract Well-adherent amine-functionalized porous silica films have been deposited on gold electrodes by combining the self-assembly technology, the sol,gel process, and the electrochemical modulation of pH at the electrode/solution interface. A partial self-assembled monolayer of mercaptopropyl-trimethoxysilane (MPTMS) was first formed on disposable gold electrodes from recordable CDs (Au-CDtrodes). The so pretreated MPTMS-Au-CDtrodes were immersed in a stable sol solution (pH,3) containing (3-aminopropyl)-triethoxysilane (APTES) and tetraethoxysilane (TEOS). Polycondensation of the APTES and TEOS precursors was then achieved by applying a negative potential for a given period of time to generate a local pH increase at the electrode/solution interface and promote the deposition of the amine functionalized silica film adhering well to the electrode surface owing to the MPTMS monolayer acting somewhat as a "molecular glue". Various parameters affecting the electrodeposition process have been studied and the film permeability to redox probes in solution was characterized by cyclic voltammetry. The amine-functionalized silica film electrodes were then applied to the preconcentration of copper(II) species prior to their electrochemical detection by anodic stripping differential pulse voltammetry. Getting high sensitivity has however required the application of an electrochemical pre-activation step as the majority of the organo-functional groups were in the form of ammonium moieties (because the film was prepared from an acidic sol). This was achieved by applying a sufficiently negative potential to the electrode surface to reduce protons and increase consequently the amine-to-ammonium ratio within the film and, thus, the efficiency of the precocentration process. The resulting device was then optimized for copper(II) determination in hydroalcoholic medium, giving rise to a linear response in the 0.1,10,,M concentration range. [source] Trace Determination of Chromium by Square-Wave Adsorptive Stripping Voltammetry on Bismuth Film ElectrodesELECTROANALYSIS, Issue 21 2004Eleni Chatzitheodorou Abstract This works reports the use of adsorptive stripping voltammetry (AdSV) for the trace determination of chromium on a rotating-disk bismuth-film electrode (BFE). During the reductive accumulation step, all the chromium species in the sample were reduced to Cr(III) which was complexed with cupferron and the complex was accumulated by adsorption on the surface of a preplated BFE. The stripping step was carried out by using a square-wave (SW) potential-time voltammetric signal. Electrochemical cleaning of the bismuth film was employed, enabling the same bismuth film to be used for a series of measurements in the presence of dissolved oxygen. The experimental variables as well as potential interferences were investigated and the figures of merit of the method were established. Using the selected conditions, the 3, limit of detection for chromium was 100,ng L,1 (for 120,s of preconcentration) and the relative standard deviation was 3.6% at the 2,,g L,1 level (n=8). Finally, the method was applied to the determination of chromium in real samples with satisfactory results. [source] Selective Electrochemical Analysis of Various Metal Ions at an EDTA Bonded Conducting Polymer Modified ElectrodeELECTROANALYSIS, Issue 16 2004Aminur Rahman Abstract An EDTA-bonded conducting polymer modified electrode was prepared and characterized by FT-IR. The modified electrode was used for the selective electrochemical analysis of various trace metal ions such as, Cu(II), Hg(II), Pb(II), Co(II), Ni(II), Fe(II), Cd(II), and Zn(II) at the different pHs by linear sweep and square wave voltammetry. Dynamic ranges were obtained using square wave voltammetry from 0.1,,M to 10.0,,M for Co(II), Ni(II), Cd(II), Fe(II), and Zn(II) and 0.5,nM to 20,nM for Cu(II), Hg(II), and Pb(II) after 10,min of preconcentration. The detection limits were determined to be 0.1,nM, 0.3,nM, 0.4,nM, 50.0,nM, 60.0,nM, 65.0,nM, 80.0,nM, and 90.0,nM for Cu(II), Hg(II), Pb(II), Co(II), Ni(II), Cd(II), Fe(II), and Zn(II), respectively. The technique offers an excellent way for the selective trace determination of various heavy metal ions in a solution. [source] Total analysis of endocrine disruptors in a microchip with gold nanoparticlesELECTROPHORESIS, Issue 18 2010Hui-Bog Noh Abstract The development of a simple, sensitive, and direct method for the total analysis of certain endocrine disruptors was performed by integrating preconcentration steps to a separation step on a microchip through the modification of the field-amplified sample stacking and field-amplified sample injection steps. To improve the preconcentration and separation performances, the preconcentration and separation buffers were modified with citrate-stabilized gold nanoparticles (AuNPs). For the detection of the separated samples, cellulose-dsDNA/AuNPs-modified carbon paste electrodes were used at the channel end. The experimental parameters affecting the analytical performances, such as the buffer concentration, water plug length, SDS concentration in the separation buffer, AuNPs concentration, preconcentration time, detection potential and electrode to channel distance, were examined. The detection limits of the test compounds were between 7.1 and 11.1,fM and that for 4-pentylphenol was 7.1 (±1.1) fM. Dynamic ranges were in the range from 0.15 to 600.0,pM. The experiments with real samples were performed to evaluate the reliability of the proposed method. [source] Cover Picture: Electrophoresis 16'2010ELECTROPHORESIS, Issue 16 2010Article first published online: 19 AUG 2010 Issue no. 16 is a regular issue with an Emphasis on "Proteins and Proteomics" comprising 20 manuscripts distributed over 4 separate parts. Part I has 7 research articles on various aspects of proteins and proteomics including combinatorial peptide ligand library for accessing low abundance proteins, analysis of membrane proteins, proteomic profiling of human colon cancer cells, quantitative determinations of biomarkers in clinical diagnostics, recombinant factor VIII, analysis of E. coli soluble proteins, and a weakly basic amino-reactive fluorescent label for IEF of proteins and chip electrophoresis. Part II has 2 research articles dealing with the CE analysis of magnetic nanoparticles and a microfluidic magnetic bead impact for cell stimulation. Part III consists of 2 research articles dealing with on-line preconcentration in CE. Instrumentation, devices and various methodologies are described in 9 research articles, which make the content of Part IV. Featured articles include: Combinatorial peptide ligand library plasma treatment: Advantages for accessing low-abundance proteins ((doi: 10.1002/elps.201000188)) Precautions to improve the accuracy of quantitative determinations of biomarkers in clinical diagnostics ((doi: 10.1002/elps.201000243)) Rapid identification of Candida albicans in blood by combined capillary electrophoresis and fluorescence in situ hybridization ((doi: 10.1002/elps.201000138)) [source] Study of electromigration effects on a pH boundary during the on-line electrokinetic preconcentration by capillary electrophoresisELECTROPHORESIS, Issue 16 2010ina Vítková Abstract A contribution to the description of electrokinetic effects on the pH boundary formed by sodium borate pH 9.5 and sodium phosphate pH 2.5 electrolytes for on-line preconcentration of weak acids is presented in this article. Simulations of electrokinetic injections together with experimental studies using contactless conductivity detection verified that the preconcentration is induced mainly by dissociation changes of analytes on the pH boundary and transient ITP state. Moreover, a study of the addition of organic solvent to the injection electrolyte was performed with impressive results. Subnanomolar LODs of hydroxybenzoic acids were achieved with 80% of methanol in the injection electrolyte which represents more than 70,000-fold preconcentration in comparison with classical CZE method. [source] Electrokinetic supercharging-electrospray ionisation-mass spectrometry for separation and on-line preconcentration of hypolipidaemic drugs in water samplesELECTROPHORESIS, Issue 7 2010Mohamed Dawod Abstract Electrokinetic supercharging, a powerful on-line preconcentration technique in CE, was for the first time hyphenated with ESI-MS for the on-line concentration and separation of five hypolipidaemic drugs. The electrophoretic separation was performed in a co-EOF mode using the EOF reversal agent, hexadimethrine bromide, in ammonium bicarbonate electrolyte, pH 9.00. The ionic strength and the amount of methanol in the buffer were optimised in a multivariate manner using artificial neural networks, with the optimal conditions being 60,mM ammonium bicarbonate containing 60% methanol, providing baseline resolution of the five hypolipidaemics within 20,min. Using electrokinetic supercharging, the sensitivity of the method was improved 1000-fold over a conventional injection under field-amplified sample stacking conditions with LODs of 180,ng/L. This is the first report of the separation of hypolipidaemics by CE. The developed method was validated and then applied to the determination of the target drugs in water samples from Hobart city. [source] Heart-cutting 2D-CE with on-line preconcentration for the chiral analysis of native amino acidsELECTROPHORESIS, Issue 6 2010Suzanne Anouti Abstract The use of transient moving chemical reaction boundary (tMCRB) was investigated for the on-line preconcentration of native amino acids in heart-cutting 2D-CE with multiple detection points using contactless conductivity detection. The tMCRB focusing was obtained by using ammonium formate (pH 8.56) as sample matrix and acetic acid (pH 2.3) as a BGE in the first dimension of the heart-cutting 2D-CE. Different experimental parameters such as the injected volume and the concentration in ammonium formate were optimized for improving the sensitivity of detection. A stacked fraction from the first dimension was selected, isolated in the capillary, and then separated in the second dimension in the presence of a chiral selector ((+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid). This on-line tMCRB preconcentration coupled with heart-cutting 2D-CE was applied with success to the chiral separation of D,L -phenylalanine, and D,L -threonine in a mixture of 22 native amino acids. The sample mixture was diluted in 0.8,M of ammonium formate, and injected at a concentration of 2.5,,M for each enantiomer with a volume corresponding to 10% of the total capillary volume. An LOD (S/N=3) of 2,,M was determined for L -threonine. [source] Electric field-enhanced transport across phase boundaries and membranes and its potential use in sample pretreatment for bioanalysisELECTROPHORESIS, Issue 5 2010Pavel Kubá Abstract Separation techniques, such as electrodialysis, electroextraction, electro-membrane extraction and extraction across phase interfaces, are reviewed and discussed as methods for sample cleanup and preconcentration. This survey clearly shows that electromigration of ionic species across phase interfaces, especially across supported liquid membranes, may be very selective and is strongly dependent on the chemical composition of these interfaces. Thus, electric field-enhanced transport across chemically tailored liquid membranes may open new perspectives in preparative analytical chemistry. This review offers comprehensive survey of related literature and discussion of the topic, which may stimulate interest of experts and practitioners in bioanalysis. [source] Direct chiral analysis of primary amine drugs in human urine by single drop microextraction in-line coupled to CEELECTROPHORESIS, Issue 16 2009Kihwan Choi Abstract Three-phase single drop microextraction (SDME) was in-line coupled to chiral CE of weakly basic amine compounds including amphetamine. SDME was used for the matrix isolation and sample preconcentration in order to directly analyze urine samples with the minimal pretreatment of adding NaOH. A small drop of an acidic aqueous acceptor phase covered with a thin layer of octanol was formed at the tip of a capillary by simple manipulation of the liquid handling functions of a commercial CE instrument. While the saline matrix of the urine sample was blocked by the octanol layer, the basic analytes in a basic aqueous donor phase were concentrated into the acidic acceptor drop through the octanol layer by the driving force of the pH difference between the two aqueous phases. The enantiomers of the enriched amines were resolved by using (+)-(18-crown-6)-tetracarboxylic acid as a chiral selector for the subsequent CE separation. From 10,min SDME with the agitation of the donor phase by a small stirrer retrofit to the CE instrument, enrichment factors were about a 1000-fold, yielding the LOD of 0.5,ng/mL for amphetamine. This low LOD value as well as the convenience of in-line coupled SDME make the proposed scheme well suited for the demanding chiral analysis of amphetamine-type stimulants. [source] Cover Picture: Electrophoresis 13'09ELECTROPHORESIS, Issue 13 2009Article first published online: 20 JUL 200 Issue 13 is a special issue on "CE and CEC of Amino Acids, Peptides and Proteins" assembling 19 papers on various topics including fast, high efficient and high sensitive "CE and CEC techniques for quality control and purity determination of native and (bio)synthetic amino acids, peptides and proteins, for monitoring of their synthesis, isolation, chemical derivatization and enzymatic digestion and also for investigation of their interactions with other molecules. New methodologies, such as electrodialysis for sample preparation, chiral ligand-exchange CE, immunoaffinity CE, affinity capillary isoelectric focusing, combination of transient isotachophoretic preconcentration with capillary zone electophoresis (CZE) analysis, two-dimensional CE-mass spectrometry (MS) separations and advances in high-sensitive CE-laser induced fluorescence (LIF) and CE-electrochemiluminescence detection schemes, are widely presented here. The applications of CE and CEC methods include chiral analysis of amino acids, determination of low abundant amino acids, peptides and proteins in complex matrices, such as human and animal body fluids and tissue biopsies, and profiling of cell lysates and recombinant proteins, e.g. birch pollen allergen and human interleukin 7. As can be seen from several contributions, preparation of new capillary coatings suppressing the adsorption of peptides and proteins to the fused silica capillary wall in their CZE analyses and/or increasing the selectivity of their open-tubular CEC separations remains a hot topic in the area of CE and CEC developments. In addition, it is shown that through the theoretical modelling of the CZE determined effective electrophoretic mobilities of proteins, the important parameters, such as charge, hydration and shape of their molecules, can be estimated." [source] Cover Picture: Electrophoresis 11'09ELECTROPHORESIS, Issue 11 2009Article first published online: 10 JUN 200 Issue no. 11 is a regular issue consisting of 22 research articles distributed over 5 parts including: (i) Proteins and Proteomics, (ii) EKC and CEC, (iii) Detection and Preconcentration Approaches, (iv) Enantioseparation and (v) Methodologies and Assays. Selected articles are: Quantifying Western blots: pitfalls of densitometry ((10.1002/elps.200800720)) Light emitting diode-induced chemiluminescence detection for capillary electrophoresis ((10.1002/elps.200800708)) Double sample preconcentration by in-line coupled large volume single drop microextraction and sweeping in capillary electrophoresis ((10.1002/elps.200800759)) [source] On-line preconcentration and enantioseparation of thalidomide racemates by CEC with the hyphenation of octyl and norvancomycin monolithsELECTROPHORESIS, Issue 4 2009An-Na Tang Abstract A method was developed for simultaneous preconcentration and chiral separation of thalidomide enantiomers in human urine by CEC in combination with self-concentration and solvent gradient effects. A 4,cm long octyl (C8) monolithic column was hyphenated with a 15,cm long norvancomycin (NVC)-bonded monolithic column via a fluorinated ethylene,propylene interface. Sample solution was injected into the C8 monolithic column, the two thalidomide enantiomers were first preconcentrated on the C8 monolithic column, and then separated with a further concentration on the NVC-bonded monolithic column by CEC. Injection of 34.8,mm plug of sample solution gave 278- and 298-fold enhancement in sensitivity, and detection limits of 90 and 94,,g/L for the two thalidomide enantiomers. Peak areas of the two isomers were linear in a range of 0.5,50,mg/L. The precision for five replicate injections of 10,mg/L were 0.8,0.9 and 1.1,2.3% for the migration time and peak height, respectively. The developed method was applied to the determination of racemic thalidomide in spiked human urine samples. [source] Novel negatively charged tentacle-type polymer coating for on-line preconcentration of proteins in CEELECTROPHORESIS, Issue 4 2009Liang Xu Abstract A novel negatively charged tentacle-type polymer-coated capillary column was fabricated and applied for on-line extraction and preconcentration of proteins. The polymer coating was prepared by glycidyl-methacrylate graft polymerization in a silanized capillary column and the following sulfonic acid group functionalization. It had high surface area and offered high phase ratio for protein adsorption. In addition, the polymer-coated capillary column provided more stable EOF than a bare uncoated capillary. These features of the polymer coating facilitated the extraction of proteins through electrostatic interactions. This was used to extract proteins. The extracted analytes were then desorbed and focused by EOF in the direction opposite to the sample injection flow for subsequent CE. With this procedure, over 1500-fold sensitivity enhancement was realized for myoglobin (MB) as compared with a normal capillary zone electrophoresis. By comparison of the peak areas of the enriched protein, it was found that the polymer-coated column could capture proteins about 30 times more than the uncoated column. In addition, the separation of a protein mixture containing 0.4,,g/mL of MB and 0.4,,g/mL of insulin was demonstrated by the on-line preconcentration and electrophoretic separation with the polymer-coated column. [source] Integrated microdevice for preconcentration and separation of a wide variety of compounds by electrochromatographyELECTROPHORESIS, Issue 3 2009Gaelle Proczek Abstract An integrated microdevice was developed to couple on-chip SPE to separation by channel electrochromatography. An acrylate-based monolith was synthesized within a glass microdevice by photoinitiated polymerization. It was used for both separation and preconcentration by direct injection on the head of the stationary phase or by confining the preconcentration step in a given zone of the stationary phase. The composition of the polymerization mixture was chosen to achieve a monolithic material containing both hydrophobic and charged moieties to ensure an electroosmotic flow for separation. As a consequence the extraction procedure occurs via hydrophobic and ionic interactions. Neutral, ionizable and charged compounds were successfully preconcentrated and separated within the microdevice through electrochromatographic mechanisms, highlighting the versatility of this device. The performance of the integrated microdevice was demonstrated with the preconcentration and separation of a mixture of PAHs for which a signal enhancement factor (SEF) of 270 was achieved within 120,s of preconcentration. In the case of charged and ionizable compounds, according to the electrolyte composition, contributions of both reverse-phase and ion-exchange mechanisms were used to perform effective electrochromatographic preconcentration. A SEF of 250 was obtained for the model-charged compound within 20,s of preconcentration. Finally, the potentials of on-chip preconcentrate and separate both neutral and ionized compounds have been demonstrated using a mixture of model compounds. [source] The combination of flow injection with electrophoresis using capillaries and chipsELECTROPHORESIS, Issue 1 2009Wen-juan Lü Abstract The technique of combined flow injection CE (FI-CE) integrates the essential favorable merits of FI and CE. It utilizes the various excellent on-line sample pretreatments and preconcentration (such as cloud point extraction, SPE, ion-exchange, dynamic pH junction and head-column field-amplified sample stacking technique) of FI, which has the advantages of high speed, accuracy, precision and avoiding manual handling of sample and reagents. Therefore, the coupling of FI-CE is an attractive technique; it can significantly expand the application of CE and has achieved many publications since its first appearance. The basic principles, instrumental developments and applications of FI-CE system from 2006 to 2008 are reviewed. [source] Affinity monolith preconcentrators for polymer microchip capillary electrophoresisELECTROPHORESIS, Issue 16 2008Weichun Yang Abstract Developments in biology are increasing demands for rapid, inexpensive, and sensitive biomolecular analysis. In this study, polymer microdevices with monolithic columns and electrophoretic channels were used for biological separations. Glycidyl methacrylate- co -ethylene dimethacrylate monolithic columns were formed within poly(methyl methacrylate) microchannels by in situ photopolymerization. Flow experiments in these columns demonstrated retention and then elution of amino acids under conditions optimized for sample preconcentration. To enhance analyte selectivity, antibodies were immobilized on monoliths, and subsequent lysozyme treatment blocked nonspecific adsorption. The enrichment capability and selectivity of these affinity monoliths were evaluated by purifying fluorescently tagged amino acids from a mixture containing green fluorescent protein (GFP). Twenty-fold enrichment and 91% recovery were achieved for the labeled amino acids, with a >25,000-fold reduction in GFP concentration, as indicated by microchip electrophoresis analysis. These devices should provide a simple, inexpensive, and effective platform for trace analysis in complex biological samples. [source] Coupling of solid-phase microextraction continuous bed (monolithic) capillaries with capillary zone electrophoresis for direct analysis of drugs in biological fluids,ELECTROPHORESIS, Issue 8 2008Reda Jarmalavi Abstract Hyperlink robust biocompatible solid-phase microextraction (SPME) devices were prepared using continuous bed (monolithic) restricted-access media (RAM) as the SPME capillary insert. The RAM-based SPME approach was able to simultaneously separate proteins from a biological sample, while directly extracting the active components of caffeine, paracetamol and acetylsalicylic acid from the drug NeoCitramonum. The devices were interfaced with a CZE system and fully automated analysis for sample preconcentration, desorption, separation and quantification of analytes was evaluated. Comparative study of in-line coupled SPME,CZE using RAM and RP capillary inserts was carried out. Using an SPME (RAM) insert, the calculated caffeine, paracetamol and acetylsalicylic acid LODs in a bovine plasma sample were 0.3, 0.8 and 1.9,ng/mL, respectively. [source] Electrokinetic supercharging for highly efficient peptide preconcentration in capillary zone electrophoresisELECTROPHORESIS, Issue 7 2008Jean-Marc Busnel Abstract Electrokinetic supercharging has been integrated in CZE for the development of a highly sensitive methodology for protein tryptic digest analysis. A careful choice of the experimental conditions led to sensitivity enhancement factors between 1000 and 10,000 whilst maintaining a satisfactory resolution. Peptides in the low nanomolar concentration range have been detected despite the use of the poorly sensitive UV absorbance detection mode. The buffer system used in this study is fully suitable for coupling CE to MS. [source] | ||||||||||||||||||||||