• Title/Summary/Keyword: capillary electrophoresis (CE)

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Enantioselective electrophoretic behavior of lipoic acid in single and dual cyclodextrin systems

  • Le, Thi-Anh-Tuyet;Nguyen, Bao-Tan;Phan, Thanh Dung;Kang, Jong-Seong;Kim, Kyeong Ho
    • Analytical Science and Technology
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    • v.34 no.4
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    • pp.143-152
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    • 2021
  • Capillary electrophoresis (CE) is an effective technique to study chiral recognition because it offers flexibility in adjusting vital factors. Currently, various available cyclodextrins (CDs) can be employed for the chiral separation of numerous analytes. Herein, we investigate the enantioseparation behavior of lipoic acid enantiomers in various types of single and dual CD systems through CE. Additionally, several impacted CE parameters were optimized through the systematic investigation based on the design of experiment (DoE) concept for a single system comprising a heptakis (2,3,6-tri-O-methyl)-β-CD and a dual system containing the combination of the single CD with a sulfated-β-CD. Consequently, absolute enantioresolution was obtained within 15 min on a common standard bare fused-silica capillary (64.5/56 cm in total/effective length, 50/365 ㎛ inner/outer diameter), maintained at 15 ℃ and at an applied voltage of 24 kV. The optimal background electrolyte consisted of 6 mM heptakis (2,3,6-tri-O-methyl)-β-CD dissolved in the solution of 58 mM borate buffer at pH 10. Furthermore, the results of apparent binding constant experiments indicated that the S-enantiomer-heptakis (2,3,6-tri-O-methyl)-β-CD complex exhibited a stronger affinity than its R-enantiomer counterpart. The obtained electrophoretic mobility values could be utilized to interpret the resolution achieved at various CD concentrations and the mobility behavior of the complexes elucidated the migration order of the enantiomers in an electropherogram.

Investigation of Enantiomer Separation Using Chiral Crown Ethers as Chiral Selectors

  • Lee, Wonjae
    • Journal of Integrative Natural Science
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    • v.9 no.1
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    • pp.28-34
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    • 2016
  • A number of chiral selectors have been developed and applied for enantiomer separation of a variety of chiral compounds. Among these chiral selectors are chiral crown ethers, a class of synthetic host polyether molecules that bind protonated chiral primary amines with high selectivity and affinity. In this paper, two important chiral crown ethers as chiral selectors of bis-(1,1'-binaphthyl)-22-crown-6 and (18-crown-6)-2,3,11,12-tetracarboxylic acid (18-C-6-TA) are focused. They have been widely used to resolve the enantiomers of chiral compounds containing a primary amino moiety using chiral stationary phases (CSPs) or chiral selectors by high-performance liquid chromatography (HPLC), capillary electrophoresis (CE) and so on in chirotechnology. Also, it was described that the commercially available covalent type HPLC CSPs derived from (+)- and (-)-18-C-6-TA have been developed and successfully applied for the resolution of various primary amino compounds including amino acids.

Determination of Terbutaline Enantiomers in Human Urine by Capillary Electrophoresis Using $Hydroxypropyl-{\beta}-cyclodextrin$ as a Chiral Selector

  • Kim, Kyeong-Ho;Seo, Sang-Hun;Kim, Hyun-Ju;Jeun, Eun-Young;Kang, Jong-Seong;Mar, Woong-Chon;Youm, Jeong-Rok
    • Archives of Pharmacal Research
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    • v.26 no.2
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    • pp.120-123
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    • 2003
  • A method for the determination of terbutaline enantiomers in human urine by capillary elctrophoresis has been developed. Optimum resolution was achieved using 50 mM phosphate buffer, pH 2.5, containing 15 mM of hydroxypropyl-$\beta$-cyclodextrin as a chiral selector. Urine samples were prepared by solid-phase extraction with Sep-pak silica, followed by CE. The assay was linear between 2-250 ng/mL (R = 0.9998 for (S)-(+)-terbutaline and R = 0.9999 for (R)-(-)-terbutaline) and detection limit was 0.8 ng/mL. The intra-day variation ranged between 6.3 and 14.5% in relation to the measured concentration and the inter-day variation was 8.2-20.1%. It has been applied to the determination of (S)-(+)-terbutaline and (R)-(-)-terbutaline in urine from healthy volunteer dosed with racemic terbutaline sulfate.

Simultaneous Detection of 10 Foodborne Pathogens using Capillary Electrophoresis-Based Single Strand Conformation Polymorphism

  • Oh, Mi-Hwa;Hwang, Hee-Sung;Chung, Bo-Ram;Paik, Hyun-Dong;Han, Sang-Ha;Kang, Sun-Moon;Ham, Jun-Sang;Kim, Hyoun-Wook;Seol, Kuk-Hwan;Jang, Ae-Ra;Jung, Gyoo-Yeol
    • Food Science of Animal Resources
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    • v.32 no.2
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    • pp.241-246
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    • 2012
  • This report outlines the development of a rapid, simple, and sensitive detection system for pathogenic bacteria using a capillary electrophoresis-based, single strand conformation polymorphism (CE-SSCP) combined with PCR. We demonstrate that this method, used with primers targeting the V4 region of the16S rRNA gene, is capable of the simultaneous detection of 10 microbes that could be associated with foodborne illness, caused by animal-derived foods: Salmonella enterica, Listeria monocytogenes, Escherichia coli O157:H7, Campylobacter jejuni, Staphylococcus aureus, Bacillus cereus, Clostridium perfringens, Yersinia enterocolitica, Vibrio parahaemolyticus, and Enterobacter sakazakii. The traditional detection techniques are time-consuming and labor-intensive, due to the necessary task of separate cultivation of each target species. As such, the CE-SSCP-PCR method, that we have developed, has the potential to diagnose pathogens rapidly, unlike the traditional technique, in order to prevent foodborne illness in a much more efficient manner.

Detection of Simazine, Atrazine and Ametryn Herbicides on a Microfluidic Chip Based on CE-AD (CE-AD기반의 Microfluidic chip을 이용한 Simazine과 Atrazine 그리고 Ametryn Herbicides의 검출)

  • Islam, Kamrul;Jang, You-Cheol;Chand, Rohit;Jha, Sandeep Kumar;Kim, Yong-Sang
    • Proceedings of the KIEE Conference
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    • 2011.07a
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    • pp.1688-1689
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    • 2011
  • A simple and rapid capillary electrophoresis method was developed for the quantitative analysis of common triazine herbicides. Cyclic voltammetry was employed to clarify the detection voltage which showed characteristic irreversible cathodic peaks. For the analysis, the mixture of triazine herbicides was applied in a microfluidic chip to determine the CE-separated peaks. Soil sample extracts were analyzed directly after drying and redissolution with the supporting electrolyte but without other pretreatment. The results were comparable to those obtained by HPLC with UV detection. Therefore, this method can be used in the rapid determination of pesticide/herbicide residues.

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An Electrochemical Detector Using Prussian Blue Electrodeposited Indium Tin Oxide Electrode (Prussian blue가 전착된 indium tin oxide 전극을 이용한 전기화학적 검출기)

  • Yi, In-Je;Kim, Ju-Ho;Kang, Chi-Jung;Kim, Yong-Sang
    • The Transactions of the Korean Institute of Electrical Engineers C
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    • v.54 no.10
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    • pp.449-452
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    • 2005
  • We fabricated an electrochemical detector (ECD) to catalyze redox reaction efficiently by electrodepositing Prussian blue (PB) on the indium tin oxide (ITO) electrode. Capillary electrophoresis (CE) and amperometric method were used. We investigated the PB surface properties by topography from atomic force microscopy (AFM). Also PB film thickness calibration with respect to deposition time and voltage was used to get better PB surFace. The PB thin film of dense and smooth surface could catalyze redox reaction efficiently. Comparing with CE-ECD microchip using bare-lTO electrode, proposed CE-ECD microchip using PB deposited electrode has shown better sensitivity by determining the detected peak current from the electropherograms while the concentration of tested analyzes was maintained the same. It is verified that detection limit can be lowered for 0.01 mM of dopamine and catechol respectively.

Analysis of the Metabolites of 1,2,4-Trimethylbenzene by Capillary Electrophoresis (모세관 전기영동법을 이용한 1,2,4-트리메틸벤젠 대사체의 분석)

  • Kang, Jong-Seong;Hong, Cheong-Hee;Lim, Jeong-Mi;Lee, Yong-Moon;Jang, Jae-Yeon
    • Analytical Science and Technology
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    • v.12 no.4
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    • pp.326-331
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    • 1999
  • The metabolites of 1,2,4-trimethylbenzene (TMB) were synthesized and determined by capillary electrophoresis (CE). The optimum conditions of CE for the separation and determination of 3,4-, 2,4-, 2,5-dimethylbenzoic acid and 3,4-, 2,4-, 2,5-dimethylhippuric acid from the rat urine were as following: the fused silica capillary($75{\mu}m$ i.d. ${\times}$ 36 cm length, 29 cm to detector) was used and kept at $15^{\circ}C$. The applied voltage was 10㎸ and compounds were detected at UV 210 mnm and 254 nm. The running electrolyte was 0.1 M phosphate buffer (pH 7) containing 15 mM of ${\beta}-CD$ and 3% of 2-propanol. The relative amount of the metabolite of 1,2,4-TMB in the rat urine was 56.7% of 3,4-isomer, 30.5% of 2,4-isomer and 12.8% of 2,5-isomer. This method can be applied to the analysis of TMB-metabolites in human urine.

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NEAR INFRARED TRANSFLECTANCE SPECTROSCOPY (NIRS) IN PHYTOCHEMISTRY

  • Huck, C.W.;W.Guggenbichler;Bonn, G.K.
    • Proceedings of the Korean Society of Near Infrared Spectroscopy Conference
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    • 2001.06a
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    • pp.3114-3114
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    • 2001
  • During the last years phytochemistry and phytopharmaceutical applications have developed rapidly and so there exists a high demand for faster and more efficient analysis techniques. Therefore we have established a near infrared transflectance spectroscopy (NIRS) method that allows a qualitative and quantitative determination of new polyphenolic pharmacological active leading compounds within a few seconds. As the NIR spectrometer has to be calibrated the compound of interest has at first to be characterized by using one or other a combination of chromatographic or electrophoretic separation techniques such as thin layer chromatography (TLC), high performance liquid chromatography (HPLC), capillary electrophoresis (CE), gas chromatography (GC) and capillary electrochromatography (CEC). Both structural elucidation and quantitative analysis of the phenolic compound is possible by direct coupling of the mentioned separation methods with a mass spectrometer (GC-MS, LC-MS/MS, CE-MS, CEC-MS) and a NMR spectrometer (LC-NMR). Furthermore the compound has to be isolated (NPLC, MPLC, prep. TLC, prep. HPLC) and its structure elucidated by spectroscopic techniques (UV, IR, HR-MS, NMR) and chemical synthesis. After that HPLC can be used to provide the reference data for the calibration step of the near infrared spectrometer. The NIRS calibration step is time consuming, which is compensated by short analysis times. After validation of the established NIRS method it is possible to determine the polyphenolic compound within seconds which allows to raise the efficiency in quality control and to reduce costs especially in the phytopharmaceutical industry.

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모세관 전기이동을 이용한 ${\delta}$-Aminolevulinc acid와 Porphobilinogen의 분리

  • Kim, Jin-Nam;Yun, Jong-Seon;Ryu, Hwa-Won
    • 한국생물공학회:학술대회논문집
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    • 2000.04a
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    • pp.512-515
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    • 2000
  • In this study, ${\delta}-aminolevulinic$ acid, porphobilinogen, glycine and levulinic acid were succesfully separated by capillary electrophoresis(CE). We established the separative conditions of the mixture containing four components by CE. The borate buffered solution was used for CE electrolyte, and its pH was adjusted to $9.25{\sim}9.42$. Under constant current or constant voltage, higher concentraion of borate produced better resolution of four components, but adversely affected migration rates , resulting in longer analysis time. While migration time was faster with increase in applied voltage, but adversely affected resolution. Each component was separated well in borate buffer of 30mM at the applied voltage of 20kV.

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Chiral Separation of Quinolone Antibacterial Agent by Capillary Electrophoresis (모세관 전기 영동을 이용한 퀴놀린계 항생제의 광학 이성질체 분석)

  • Gang, Dae Cheon;Jo, Seung Il;Jeong, Du Su;Choe, Gyu Seong;Kim, Yong Seong
    • Journal of the Korean Chemical Society
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    • v.46 no.5
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    • pp.412-429
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    • 2002
  • Chiral separation of gemifloxacin, an quinolone antibacterial agent, using (+)-(18-crown-6)-tetracar-boxylic acid $(18C6H_4)$ as a chiral selector was performed by capillary electrophoresis (CE). Direct analysis of quinolone antibacterial agent in body fluid is beneficial in terms of fast analysis time, multicomponent analysis. However, high con-centration of sodium ion in body fluid can prevent gemifloxacin from interacting with $18C6H_4$ since sodium ion has high affinity with $18C6H_4$ due to the strong charge interaction. Ethylenediaminetetraacetic acid (EDTA), as a chelating ligand, was added in the running buffer in order to reduce the interaction between sodium ion and the chiral selector. Increased separation efficiency and reduced migration time were observed while sodium ion exists in the sample solution at the concentration up to 150 mM.