Home About us Contact
|
Home About us Contact | ||
|
|
||
Micellar Electrokinetic Chromatography (micellar + electrokinetic_chromatography)
Selected AbstractsSeparation and Detection of Narcotic Drugs on a Microchip Using Micellar Electrokinetic Chromatography and ElectrochemiluminescenceELECTROANALYSIS, Issue 6 2008Yan Du Abstract A new approach for fast and sensitive electrochemiluminescence (ECL) detection of narcotic drugs on a microchip after separation by micellar electrokinetic chromatography (MEKC) is presented, taking the cocaine and its hydrolysate ecgonine as the test analytes. The mixture of hydrophilic BMIMBF4 ionic liquid (IL) and sodium dodecyl sulfate (SDS) was used directly as the buffer of MEKC with less noisy baselines, lower electrophoretic current and satisfactory separation performance. This developed microchip MEKC,ECL system was successfully applied to the determination of two very similar narcotics, heroin and codeine, within 100s in urine sample and was demonstrated as a promising method in clinical and forensic analysis. [source] Detection of chlorinated quinones using interdigitated electrodes coupled with capillary electrophoresisELECTROPHORESIS, Issue 6 2003Keith B. Male Abstract An array of eight interdigitated microband gold electrodes (IDEs) has been developed together with electrophoretic separation for analysis of chlorinated hydroquinones (ClHQs) and benzoquinones (ClBQs). The IDE chip positioned very close to the separation capillary outlet served as an amplification/detection system without the requirement for frequent "capillary-electrode" alignment. ClHQs, electrophoretically migrating to the IDE surface, were oxidized at +1.1 V by seven electrodes of the array and then detected by the remaining electrode, poised at ,0.1 V. Conversely, ClBQs were detected at +1.1 V by the detecting electrode after having been reduced at the 7 adjacent electrodes poised at ,0.1 V. There was an amplification effect on both the detecting electrode as well as the adjacent electrodes because of the recycle between ClHQs and ClBQs. The detecting "amplification" current response was dependent on the potentials applied, the position of the detecting electrode on the array, the number of adjacent electrodes being used for recycling and the distance between the oxidative and reductive electrodes. Micellar electrokinetic chromatography (MEKC) separation of the analytes was achieved using 30 mM sodium dodecyl sulfate (SDS) with a detection limit in the range of 2,20 ,M. In addition to a facile "capillary-electrode" alignment, the important aspect described here was the capability of detecting through recycling a reduced compound (in the case of ClHQs) at a negative potential to circumvent fouling and electroactive interferences. An appealing feature was also the concurrent oxidation/reduction detection for each compound to ascertain peak assignment, as interfering compounds are less likely to exhibit the same oxidative/reductive characteristics and electrophoretic mobilities as the target analytes. [source] Analysis of glycopeptide antibiotics using micellar electrokinetic chromatography and borate complexationBIOMEDICAL CHROMATOGRAPHY, Issue 2-3 2003Carmelle Lucas Abstract Micellar electrokinetic chromatography (MEKC) was investigated as a technique for the separation and analysis of the following related glycopeptide antibiotics: ,-avoparcin, ,-avoparcin, ristocetin A, ristocetin B and vancomycin. Sodium dodecyl sulfate (SDS) micelles were employed as the pseudostationary phase in conjunction with borate or CHES buffers at pH 9.2. A complete separation of the glycopeptides was achieved only when two separation mechanisms were employed simultaneously: (i) differential partitioning of the glycopeptides into SDS micelles; and (ii) differential complexation of the glycopeptides with the borate anion from the borate buffer. Quantitatively, linearity was confirmed for each antibiotic from 0.5 to 40,ppm, with correlation coefficients (r2) ranging from 0.9996 (vancomycin and ,-avoparcin) to 0.9986 (,-avoparcin). Detection limits ranging from 0.01,ppm (vancomycin) to 0.2,ppm (avoparcin) were achieved, and the mean recovery of avoparcin at the 10,ppm level was 99.2%. Copyright © 2003 John Wiley & Sons, Ltd. [source] RNA interference of sialidase improves glycoprotein sialic acid content consistencyBIOTECHNOLOGY & BIOENGINEERING, Issue 1 2006Frederyk A. Ngantung Abstract An important challenge facing therapeutic protein production in mammalian cell culture is the cleavage of terminal sialic acids on recombinant protein glycans by the glycosidase enzymes released by lysed cells into the supernatant. This undesired phenomenon results in a protein product which is rapidly cleared from the plasma by asialoglycoprotein receptors in the liver. In this study, RNA interference was utilized as a genetic approach to silence the activity of sialidase, a glycosidase responsible for cleaving terminal sialic acids on IFN-, produced by Chinese Hamster Ovary (CHO) cells. We first identified a 21-nt double stranded siRNA that reduced endogenous sialidase mRNA and protein activity levels. Potency of each siRNA sequences was compared using real time RT-PCR and a sialidase activity assay. We next integrated the siRNA sequence into CHO cells, allowing production and selection of stable cell lines. We isolated stable clones with sialidase activity reduced by over 60% as compared to the control cell line. Micellar electrokinetic chromatography (MEKC), thiobarbituric acid assay (TAA), and high performance anion exchange chromatography (HPAEC) coupled to amperometric detection were performed to analyze glycan site occupancy, sialic acid content, and distribution of asialo-/sialylated-glycan structures, respectively. Two of the stable clones successfully retained the full sialic acid content of the recombinant IFN-,, even upon cells' death. This was comparable to the case where a chemically synthesized sialidase inhibitor was used. These results demonstrated that RNA interference of sialidase can prevent the desialylation problem in glycoprotein production, resulting improved protein quality during the entire cell culture process. © 2006 Wiley Periodicals, Inc. [source] Separation and Detection of Narcotic Drugs on a Microchip Using Micellar Electrokinetic Chromatography and ElectrochemiluminescenceELECTROANALYSIS, Issue 6 2008Yan Du Abstract A new approach for fast and sensitive electrochemiluminescence (ECL) detection of narcotic drugs on a microchip after separation by micellar electrokinetic chromatography (MEKC) is presented, taking the cocaine and its hydrolysate ecgonine as the test analytes. The mixture of hydrophilic BMIMBF4 ionic liquid (IL) and sodium dodecyl sulfate (SDS) was used directly as the buffer of MEKC with less noisy baselines, lower electrophoretic current and satisfactory separation performance. This developed microchip MEKC,ECL system was successfully applied to the determination of two very similar narcotics, heroin and codeine, within 100s in urine sample and was demonstrated as a promising method in clinical and forensic analysis. [source] Simultaneous determination of memantine and amantadine in human plasma as fluorescein derivatives by micellar electrokinetic chromatography with laser-induced fluorescence detection and its clinical applicationELECTROPHORESIS, Issue 11 2010Hsin-Hua Yeh Abstract A nonionic surfactant MEKC method with LIF detection was developed for the simultaneous determination of memantine, an anti-Alzheimer's disease agent, and amantadine, an anti-Parkinson's disease drug, in human plasma. Before analysis, the plasma samples were pretreated by liquid,liquid extraction with ethyl acetate, and derivatized with 6-carboxyfluorescein N -hydroxysuccinimide ester. The chemical derivatization is performed with 6-carboxyfluorescein N -hydroxysuccinimide ester in ACN , 5,mM pH 9.0 borate buffer (40:60, v/v) at 35°C for 3,h. After the derivatization reaction, hydrodynamic injection (0.5,psi, 8,s) was used to introduce the derivatized solution, and the separation was performed in borate buffer (30,mM, pH 9.5) with the nonionic surfactant Brij-35® (0.07%, w/v); the separation voltage was 6,kV. The linear ranges of the method for the determination of memantine and amantadine in human plasma were over a range of 2.0,60.0,ng/mL. The detection limit was 0.5,ng/mL (S/N=3). This method was applied successfully to monitor the concentration of memantine or amantadine in patients with Alzheimer's disease or Parkinson's disease. [source] Length-dependent DNA separations using multiple end-attached peptide nucleic acid amphiphiles in micellar electrokinetic chromatographyELECTROPHORESIS, Issue 13 2008Jeffrey M. Savard Abstract End-labeled free-solution electrophoresis (ELFSE) is an alternative approach to gel-based methods for size-based electrophoretic separation of DNA. In ELFSE, an electrically neutral "drag-tag" is appended to DNA to add significant hydrodynamic drag, thereby breaking its constant charge-to-friction ratio. Current drag-tag architecture relies on covalent attachment of polymers to each DNA molecule. We have recently proposed the use of micellar drag-tags in conjunction with sequence-specific hybridization of peptide nucleic acid amphiphiles (PNAAs). This work investigates the effect of multiple PNAA attachment on DNA resolution using MEKC. Simultaneous PNAA hybridization allows for the separation of long DNA targets, up to 1012,bases, using micellar drag-tags. Each PNAA handle independently interacts with the micellar phase, reducing the overall mobility of this complex relative to individual PNAA binding. The sequence- and size-based dependence of this separation technique is maintained with multiple PNAA binding over a range of DNA sizes. Results are accurately described by ELFSE theory, yielding , = 54 for single-micelle tagging and , = 142 for dual-micelle tagging. This method is the first example of a non-covalent drag-tag used to separate DNA of 1000,bases based on both size and sequence. [source] Determination of amino acids by micellar EKC: Recent advances in method development and novel applications to different matricesELECTROPHORESIS, Issue 1 2008Paolo Iadarola Professor Abstract The extensive use of CE for the analysis of amino acids has been well documented in a series of research articles and reviews. Aim of this report is to address the attention of the reader on the recent advances of micellar electrokinetic chromatography for the separation and determination of these analytes. Enhancements in selectivity of this technique through the use of pseudostationary phases containing mixed micelles, polymers, and chiral selectors are presented. Selected applications concerning separation and quantitation of even minute amounts of amino acids in: (i) biological fluids; (ii) microdialysates; (iii) plant cells; (iv) food stuff; and (v) pharmaceutical formulations have also been covered. Advantages of MEKC over other techniques for the amino acid analysis have been underlined. [source] Rapid determination of acyclovir in plasma and cerebrospinal fluid by micellar electrokinetic chromatography with direct sample injection and its clinical applicationELECTROPHORESIS, Issue 4 2006Hsin-Hua Yeh Abstract A simple MEKC with UV detection at 254,nm for analysis of acyclovir in plasma and in cerebrospinal fluid (CSF) by direct injection without any sample pretreatment is described. The separation of acyclovir from biological matrix was performed at 25°C using a BGE consisting of Tris buffer with SDS as the electrolyte solution. Several parameters affecting the separation of the drug from biological matrix were studied, including the pH and concentrations of the Tris buffer and SDS. Using dyphylline as an internal standard, the linear ranges of the method for the determination of acyclovir in plasma and in CSF all exceeded the range of 2,50,,g/mL; the detection limit of the drug in plasma and in CSF (S/N = 3; injection 3.45,kPa, 5,s) was 1.0,,g/mL. The applicability of the proposed method for determination of acyclovir in plasma and CSF collected at 8,h after intravenous administration of 500,mg acyclovir (Zovirax®) in two patients with herpes simplex encephalitis was demonstrated. [source] Capillary electrophoresis-laser induced fluorescence analysis of endogenous damage in mitochondrial and genomic DNAELECTROPHORESIS, Issue 13 2005Michaela Wirtz Abstract Reactive oxygen molecules are formed in vivo as by-products of normal aerobic metabolism. All organisms dependent on oxygen are inevitably exposed to these species so that DNA damage can occur in both genomic and mitochondrial DNA (mtDNA). In order to determine endogenous DNA damage we have developed an analytical method that involves the isolation and hydrolysis of genomic DNA or mtDNA, the labeling of modified and unmodified nucleotides and micellar electrokinetic chromatography with laser-induced fluorescence detection. With this method we have found etheno-adenine, thymine glycol, uracil, hypoxanthine, and 5-methylcytosine. These were identified by the addition of internal standards to the genomic or mtDNA. There are a large number of other signals in the electropherograms of mtDNA that we have never found in genomic DNA analysis because they are at lower concentration in the genome. In the DNA of untreated patients with chronic lymphocytic leukemia (CLL), uracil and high levels of etheno-adenine were found, which can be explained by antioxidant enzyme alterations and oxidative stress in the CLL lymphocytes. [source] Monomeric and polymeric anionic gemini surfactants and mixed surfactant systems in micellar electrokinetic chromatography.ELECTROPHORESIS, Issue 2 2005Part II: Characterization of chemical selectivity using two linear solvation energy relationship models Abstract Sodium di(undecenyl) tartarate monomer (SDUT), a vesicle-forming amphiphilic compound possessing two hydrophilic carboxylate headgroups and two hydrophobic undecenyl chains, was prepared and polymerized to form a polymeric vesicle (i.e., poly-SDUT). The anionic surfactants of SDUT and poly-SDUT (carboxylate head group) and sodium dodecyl sulfate, SDS (sulfate head groups) as well as mixed surfactant systems (SDS/SDUT, SDS/poly-SDUT, and SDUT/poly-SDUT) were applied as pseudostationary phases in micellar electrokinetic chromatography (MEKC). Two linear solvation energy relationship (LSER) models, i.e., solvatochromic and solvation parameter models, were successfully applied to investigate the effect of the type and composition of pseudostationary phases on the retention mechanism and selectivity in MEKC. The solvatochromic and solvation parameter models were used to help understand the fundamental nature of the solute-pseudostationary phase interactions and to characterize the properties of the pseudostationary phases (e.g., solute size and hydrogen bond-accepting ability for all pseudostationary phases). The solute types were found to have a significant effect on the LSER system coefficients and on the predicted retention factors. Although both LSER models provide the same information, the solvation parameter model is found to provide much better results both statistically and chemically than the solvatochromic model. [source] Determination of the chiral and achiral related substances of methotrexate by cyclodextrin-modified micellar electrokinetic chromatographyELECTROPHORESIS, Issue 16 2004Roberto Gotti Abstract A cyclodextrin-modified micellar electrokinetic chromatographic (CD-MEKC) method for the determination of the most important potential impurities of methotrexate (MTX): 2,4-diamino-6-(hydroxymethyl)pteridine, aminopterine hydrate, 4-[N -(2-amino-4-hydroxy-6-pteridinylmethyl)- N -methylamino] benzoic acid, 4-[N -(2,4-diamino-6-pteridinylmethyl)- N -methylamino] benzoic acid, and the distomer D -MTX is presented. The MEKC separation of these compounds was optimized by applying a step-by-step approach. The addition of ,-CD to a conventional MEKC system, based on sodium dodecyl sulfate (SDS) as surfactant, showed to be essential for the enantioresolution of racemic MTX as well as for the separation of the achiral impurities. To achieve high-resolution factor between the peaks adjacent to the main component (L -MTX), as required in the analysis of related impurities, the separation conditions were stressed; in particular, the addition of methanol to the CD-MEKC system resulted in a very effective choice. Under the optimized final conditions (100 mM SDS and 45 mM ,-CD in a mixture of 50 mM borate buffer, pH 9.30-methanol (75:25 v/v)), the method was validated showing a general adequate accuracy (93,106% recovery) in the determination of L -MTX related substances at the impurity level of 0.12% w/w with a relative standard deviation (RSD)% lower than 8% (n = 4). The method was successfully applied to the analysis of pharmaceuticals (tablets and injections) which showed to contain the distomer D -MTX as major impurity and aminopterine hydrate as a further related substance in the commercial tablets. [source] Capillary electrophoresis of amphipathic ,-helical peptide diastereomersELECTROPHORESIS, Issue 1 2004Traian V. Popa Abstract We have made a rigorous assessment of the ability of capillary electrophoresis to resolve peptide diastereomers through its application to the separation of a series of synthetic 18-residue, amphipathic ,-helical monomeric peptide analogues, where a single site in the centre of the hydrophobic face of the ,-helix is substituted by 19 L - or D -amino acids. Such L - and D -peptide pairs have the same mass-to-charge ratio, amino acid sequence and intrinsic hydrophobicity, varying only in the stereochemistry of one residue. CE approaches assessed in their ability to separate diastereomeric peptide pairs included capillary zone electrophoresis (uncoated capillary), micellar electrokinetic chromatography (uncoated capillary in the presence of 3-[(3-cholamidopropyl)dimethylammonio]-1-propanesulfonate, CHAPS), open-tubular capillary electrochromatography (C8 -coated capillary in the presence of 25% 2,2,2-trifluoroethanol (TFE) or 25% ethanol). Overall, the OT-CEC methods were the most effective at separating the most peptide pairs, particularly for those containing hydrophilic side chains. However, the MEKC approach proved most effective for separation of peptide pairs containing hydrophobic or aromatic side chains. [source] In vivo simultaneous monitoring of ,-aminobutyric acid, glutamate, and L -aspartate using brain microdialysis and capillary electrophoresis with laser-induced fluorescence detection: Analytical developments and in vitro/in vivo validationsELECTROPHORESIS, Issue 18 2003Valérie Sauvinet Abstract ,-Aminobutyric acid (GABA), glutamate (Glu), and L -aspartate (L -Asp) are three major amino acid neurotransmitters in the central nervous system. In this work, a method for the separation of these three neurotransmitters in brain microdialysis samples using a commercially available capillary electrophoresis (CE) system has been developed. Molecules were tagged on their primary amine function with the fluorogene agent naphthalene-2,3-dicarboxaldehyde (NDA), and, after separation by micellar electrokinetic chromatography, were detected by laser-induced fluorescence using a 442 nm helium-cadmium laser. The separation conditions for the analysis of derivatized neurotransmitters in standard solutions and microdialysates have been optimized, and this method has been validated on both pharmacological and analytical basis. The separation of GABA, Glu, and L -Asp takes less than 10 min by using a 75 mmol/L borate buffer, pH 9.2, containing 70 mmol/L SDS and 10 mmol/L hydroxypropyl-,-cyclodextrin and +,25 kV voltage. The detection limits were 3, 15 nmol/L and, 5 nmol/L for GABA, Glu, and L -Asp, respectively. Moreover, submicroliter samples can be analyzed. This method allows a simple, rapid and accurate measurement of the three amino acid neurotransmitters for the in vivo brain monitoring using microdialysis sampling. [source] Enantioselectivity of alcohol-modified polymeric surfactants in micellar electrokinetic chromatographyELECTROPHORESIS, Issue 15 2003Jepkoech Tarus Abstract A novel method of modifying sodium undecanoyl- L -leucinate (SUL) micelles employed in chiral separation of analytes in micellar electrokinetic chromatography (MEKC) to enhance selectivity toward specific analytes is discussed. The current study aimed at modifying the SUL micelles by introducing different alcohols into the mono-SUL micelles. The micellar solutions were then polymerized in the presence of alcohols followed by postpolymerization extraction of the alcohols to yield alcohol-free polymeric surfactants (poly- L -SUL). The effects of hexanol (C6OH) and undecylenyl alcohol (C11OH) on micellar properties of this surfactant were investigated by use of surface tensiometry, fluorescence spectroscopy, pulsed field gradient-nuclear magnetic resonance (PFG-NMR), and MEKC. The surface tension and PFG-NMR studies indicated an increase in the critical micelle concentration (cmc) and micellar size upon increasing the alcohol concentration. Fluorescence measurements suggested that alcohols induce closely packed micellar structures. Coumarinic and benzoin derivatives, as well as (±)-1, 1'-binaphthyl-2,2'-dihydrogen phosphate (BNP) were used as test analytes for MEKC experiments. Examination of MEKC data showed remarkable resolutions and capacity factors of coumarinic derivatives obtained with modified poly- L -SUL as compared to the unmodified poly- L -SUL. Evaluation of fluorescence, PFG-NMR, and MEKC data suggest a strong correlation between the polarity and hydrodynamic radii of alcohol-modified micelles and the resolution of the test analytes. [source] Polymeric alkenoxy amino acid surfactants: I. Highly selective class of molecular micelles for chiral separation of ,-blockersELECTROPHORESIS, Issue 15 2003Syed A. A. Rizvi Abstract Two amino acid-based alkenoxy micelle polymers were synthesized for this study. These include polysodium N -undecenoxy carbonyl- L -leucinate (poly- L -SUCL) and polysodium N -undecenoxy carbonyl- L -isoleucinate (poly- L -SUCIL). The polymerization time and concentration of the synthesized micelle polymers were optimized by 1H-nuclear magnetic resonance (NMR) and capillary electrophoresis (CE) experiments. Detailed physicochemical properties (1H NMR, critical micelle concentration (CMC), optical rotation, partial specific volume, aggregation number, and polarity) were determined, and these molecular micelles were introduced as a pseudostationary phase in micellar electrokinetic chromatography to study the molecular recognition and to develop a method for simultaneous separation of eight chiral ,-blockers. It is found that poly- L -SUCL gives overall better chiral resolution and wider chiral window than poly- L -SUCIL. After optimizing the type of micelle polymer, injection size and temperature, simultaneous separation and enantioseparation of eight ,-blockers were achieved in less than 35 min. A comparison with the amide-type surfactants of the same polar head group and alkyl chain length showed that carbamate-type surfactants always work better than the corresponding amide-type surfactant. [source] Capillary Zone Electrophoresis and Micellar Electrokinetic Capillary Chromatography for Determining Water-Soluble Vitamins in Commercial Capsules and TabletsJOURNAL OF FOOD SCIENCE, Issue 1 2001S-C. Su ABSTRACT: A rapid method was developed for simultaneously determining thiamine, riboflavin, pyridoxine, nicotinamide, nicotinic acid, and ascorbic acid. It was tested on 15 samples. The peaks of all components were cleanly separated with good resolution by capillary zone electrophoresis (CZE) and micellar electrokinetic chromatography (MECC). CZE was performed with 0.02 M borate buffer, and MECC was performed with 4% acetonitrile in 0.02 M borate/phosphate buffer containing 0.1 M sodium dodecyl sulfate. Average recoveries for all components were 80.3% to 103.7% with coefficients of variation being less than 5%. Thiamine, nicotinic acid, and pyridoxine contents were consistent with those labeled on the packages, but nicotinamide, riboflavin, and ascorbic acid contents of some samples were less. [source] Separation of fatty alcohol ethoxylates by capillary zone electrophoresis and micellar electrokinetic chromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 3 2009Ryo Koike Abstract Separation methods based on capillary zone electrophoresis and micellar electrokinetic chromatography were developed to characterize the distribution of ethylene oxide (EO) homologues in the fatty alcohol ethoxylates (FAEs). Prior to the separation, the FAEs were derivatized with 2-fluoro-1-methylpyridinium p -toluenesulfonate (FMPTS) to allow CZE separation and UV detection. To prevent adsorption of cationic analytes onto the inner surface of the capillary and formation of micelles in CZE analysis, a lower pH background solution (BGS) containing a high concentration of acetonitrile was employed. Under optimal conditions, FMPTS-derivatized FAEs with an average EO number of 6 were completely separated within 11 min. For MEKC analysis of the FAEs, dodecyltrimethylammonium chloride (DTAC) was added to the BGS. In the presence of 30 mM DTAC in 10 mM phosphate buffer (pH 2.5) containing 20% (v/v) acetonitrile, superior oligomer separation of the FAEs containing up to 50 EO groups was achieved within 30 min with good analytical reproducibilities. Furthermore, the developed method was applied to the analysis of the FAEs in commercial products such as laundry detergent and fabric softener. [source] Separation and quantification of 9-(alkylthio)acridines by capillary micellar electrokinetic chromatography and capillary liquid chromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 13 2007Jana Nejmanová Abstract Various thioacridine derivatives are potential chemotherapeutics against various diseases which are intensively synthesized, characterized, and investigated by many research groups. Efficient, fast, and reliable separation and quantification methods for their analysis are still to be developed. MEKC and capillary LC (CLC) were applied for the separation and quantification of five highly hydrophobic, weakly basic, and structurally similar 9-(alkylthio)acridines. Since the common anionic and cationic surfactants failed to separate the strongly hydrophobic thioacridines by MEKC, sodium cholate was used in an alkaline BGE and successfully employed for their fast separation. In CLC, the weakly basic nature of the thioacridines necessitated use of LiChrosorb RP-select B sorbent as the stationary phase, which combined with a very simple mobile phase methanol/water yielded an efficient chromatographic separation system. Both, the MEKC and CLC optimized separation methods were then applied to quantify the thioacridines within a concentration range of 1.0×10,5,1.0×10,3 mol/L and the obtained experimental results were critically compared. In practical terms, the MEKC analytical method can quantify the analytes much faster but with a lower reliability while the CLC method performs slower analysis with a higher repeatability of the experimental results. [source] Determination of the purity of ampicillin by micellar electrokinetic chromatography and reversed phase liquid chromatography on a monolithic silica columnJOURNAL OF SEPARATION SCIENCE, JSS, Issue 7-8 2004Milada Dole, alová Abstract A micellar electrokinetic chromatographic (MEKC) method and a fast reversed-phase liquid chromatographic one have been developed for determining the purity of ampicillin. MEKC separation of ampicillin and its related substances was performed with the use of an untreated fused-silica capillary and 40 mM phosphate-borate buffer, pH 7.5 containing 75 mM SDS. The HPLC method employed a monolithic silica C18 column and a mobile phase composed of phosphate buffer, pH 5.2 and ACN, the flow rate being 4.0 mL/min. Both methods were successfully validated. Linearity, relative response factors, limits of quantitation, intermediate precision, and accuracy were evaluated. The methods proved to be fast, reliable, and sufficiently sensitive and, accordingly, well-suited for control of purity of ampicillin substance, injections, and capsules. A combination of both methods can be very useful in the confirmation of impurity profiles. [source] Simultaneous determination of digoxin and digitoxin by micellar electrokinetic chromatography and application to drug formulationsJOURNAL OF SEPARATION SCIENCE, JSS, Issue 18 2003Hsiu-Hui Tseng Abstract A simple micellar electrokinetic chromatographic method is described for simultaneous determination of digoxin and digitoxin. The simultaneous analysis of digoxin and digitoxin was performed in Tris buffer (10 mM; pH 9) with 90 mM sodium dodecyl sulfate and 10% isopropyl alcohol as an anionic surfactant and organic modifier. Under these conditions, good separation with high efficiency is achieved in short analysis times. Several parameters affecting the separation of the drugs were studied, including the pH and concentrations of the Tris buffer and sodium dodecyl sulfate. The linear range of the method for the determination of digoxin and digitoxin was over 0.01,0.3 mg/mL; the detection limit (signal to noise ratio = 3; injection 3.5 kPa 3 s) was 4 and 6 ,g/mL, respectively. Application of the proposed method to the determination of digoxin in commercial tablets and in injections proved to be feasible. [source] Analysis of gastrodin and tetramethylpyrazine in traditional Chinese preparations by micellar electrokinetic chromatographyJOURNAL OF SEPARATION SCIENCE, JSS, Issue 6-7 2003Wang Rongying Abstract A simple, rapid, and accurate micellar electrokinetic chromatographic method has been developed for determination of gastrodin and tetramethylpyrazine in three traditional Chinese preparations: Zhennaoning jiaonang, Yangxue shengfa jiaonang, and Xiaoshuan zaizao wan. Running buffer comprising 50 mM sodium tetraborate and 15 M sodium dodecylsulfate (SDS), pH 9.50, was found to be most suitable for the separation. All experiments was performed with a 47 cm (40 cm effective length)×75 ,m ID uncoated fused-silica capillary and UV detection at 200 nm. The linear calibration ranges were 2.5,200 ,g mL,1 (R = 0.999) for gastrodin and 5.0,200 ,g mL,1 (R = 0.997) for tetramethylpyrazine; the detection limits were 0.5 ,g mL,1 and 0.8 ,g mL,1, respectively. Recoveries of the two analytes from the samples, calculated by use of a method described in detail in the text, were between 94.21 and 104.46%. The amounts of gastrodin and tetramethylpyrazine in the preparations were easily determined within 10 min. [source] Rapid and sensitive determination of ephedrine and pseudoephedrine by micellar electrokinetic chromatography with on-line regenerating covalent coatingBIOMEDICAL CHROMATOGRAPHY, Issue 1 2005Xie Jianping Abstract A rapid, sensitive and reproducible micellar electrokinetic chromatographic method using hexamethyldisilazane as on-line regenerating covalent coating was developed for the quanti,cation of ephedrine (E) and pseudoephedrine (PE). E and PE were derivatized with 4-chloro-7-nitrobenzo-2-oxa-1,3-diazol for laser-induced ,uorescence detection. The on-line regenerating covalent coating formed a combinative double coating with the subsequently produced dynamic SDS coating. The total coating can be easily removed and conveniently regenerated on-line. The simple coating procedure was described. By a series of optimization, a running buffer of 20 mm Na2B4O7 + 16 mm SDS was applied for the separation of the derivatives. Linear relationships for E and PE were obtained in the range of 0.044,6.60 µg mL,1 (correlation coef,cients: 0.9975 for E, 0.9981 for PE), and the detection limits for E and PE were 1.71 and 0.67 ng mL,1, respectively. The separation speed, the reproducibility and the sensitivity were much improved over those of other capillary electrophoresis methods more recently reported. The method was applied to the analysis of the two alkaloids in traditional herbal preparations with recoveries in the range 92.8,104.8%. Copyright © 2004 John Wiley & Sons, Ltd. [source] Quantitation of oxcarbazepine and its metabolites in human plasma by micellar electrokinetic chromatographyBIOMEDICAL CHROMATOGRAPHY, Issue 4 2003Vincenzo Pucci Abstract A reliable micellar electrokinetic chromatographic method for the determination of oxcarbazepine and its two main metabolites, 10-hydroxycarbamazepine and 10,11- trans -dihydroxy-10,11-dihydroxycarbamazepine, in human plasma was developed. The separation and determination of the analytes was achieved using a system consisting of 60,mM SDS in phosphate buffer (30,mM, pH 8.0), to which 20% (v/v) methanol was added. Separation was carried out in an uncoated fused-silica capillary with a separation voltage of 25,kV and currents typically less than 40,µA. Spectrophotometric detection was at 205,nm. Isolation of oxcarbazepine and its metabolites from plasma was accomplished by a solid-phase extraction procedure. The mean extraction yield of the analytes from plasma was higher than 94%. The linear correlation coefficients were better than 0.994 for all analytes. The limit of detection was 0.05,µg/mL, the limit of quantitation 0.15,µg/mL. The repeatability for the spiked blank plasma samples was lower than 1.9% and the intermediate precision lower than 2.1%, both expressed as RSD%. The results obtained analysing real plasma samples from epileptic patients under therapy with Tolep® were satisfactory in terms of precision, accuracy and detectability. Copyright© 2003 John Wiley & Sons, Ltd. [source] Analysis of glycopeptide antibiotics using micellar electrokinetic chromatography and borate complexationBIOMEDICAL CHROMATOGRAPHY, Issue 2-3 2003Carmelle Lucas Abstract Micellar electrokinetic chromatography (MEKC) was investigated as a technique for the separation and analysis of the following related glycopeptide antibiotics: ,-avoparcin, ,-avoparcin, ristocetin A, ristocetin B and vancomycin. Sodium dodecyl sulfate (SDS) micelles were employed as the pseudostationary phase in conjunction with borate or CHES buffers at pH 9.2. A complete separation of the glycopeptides was achieved only when two separation mechanisms were employed simultaneously: (i) differential partitioning of the glycopeptides into SDS micelles; and (ii) differential complexation of the glycopeptides with the borate anion from the borate buffer. Quantitatively, linearity was confirmed for each antibiotic from 0.5 to 40,ppm, with correlation coefficients (r2) ranging from 0.9996 (vancomycin and ,-avoparcin) to 0.9986 (,-avoparcin). Detection limits ranging from 0.01,ppm (vancomycin) to 0.2,ppm (avoparcin) were achieved, and the mean recovery of avoparcin at the 10,ppm level was 99.2%. Copyright © 2003 John Wiley & Sons, Ltd. [source] Determination of bisphenol A and 10 alkylphenols in serum using SDS micelle capillary electrophoresis with ,-cyclodextrinBIOMEDICAL CHROMATOGRAPHY, Issue 7 2001Masatoki Katayama A new micelle capillary electrophoresis based on cyclodextrin micellar electrokinetic chromatography (MEKC) for the determination of bisphenol A and 10 alkylphenols in rat serum is reported. Several surfactants and dextrins were studied. Bisphenol A and alkylphenols were separated using a 50,µm,×,50,cm capillary with 20,mM borate phosphate buffer (pH 8.0) containing 20,mM sodium dodecylsulfate and 5,mM ,-cyclodextrin as carrier. The method could determine 0.6,2000,µg/mL of phenols in 100,µL serum by photometric detection at 214,nm. Using 2.0,mL serum, 1.0,ng/mL of phenols could be determined. The relative standards deviations were 6.3,7.7% at 10,µg/mL in serum. The recoveries were 91.8,93.0% with 10,µg/mL serum samples. Copyright © 2001 John Wiley & Sons, Ltd. [source] | |||||||||||||