• Title/Summary/Keyword: ion chromatography

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Operating Parameters for Glutamic Acid Crystallization in Displacement Ion Exchange Chromatography

  • Lee, Kisay
    • Biotechnology and Bioprocess Engineering:BBE
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    • v.2 no.2
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    • pp.117-121
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    • 1997
  • Glutamic acid can be crystallized inside cation exchange column when displacer NaOH concentration is high enough to concentrate displaced glutamic acid beyond its solubility limit. Resulting crystal layer of glutamic acid was moved with liquid phase through the column, and thus could be eluted from the column and recovered in fraction collector. For the purpose of enhancing crystal recovery, effects of operating parameters on the crystal formation were investigated. The increase in the degree of crosslinking of resin favored crystal recovery because of its low degree of swelling. Higher concentration of displacer NaOH was advantageous. If NaOH concentration is too high, however, crystal recovery was lowered due to the solubility-enhancing effects of high pH and ionic strength. The decrease of mobile phase flow rate enhanced crystal recovery because enough time to attain local equilibrium could be provided, but film diffusion would control the overall crystal formation with extremely low flow rate. Lower temperature reduced solubility of glutamic acid and thus favored crystal formation unless the rate of ion exchange was severely reduced. The ion exchange operated by displacement mode coupled with crystallization was advantageous in reducing the burden of further purification steps and in preventing purity-loss resulted from overlapping between adjacent bands.

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Determination of Co(II) Ion as a 4-(2-Thiazolylazo)resorcinol or 5-Methyl-4-(2-thiazolylazo)resorcinol Chelate by Reversed-Phase Capillary High-Performance Liquid Chromatography

  • Chung, Yong-Soon;Chung, Won-Seog
    • Bulletin of the Korean Chemical Society
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    • v.24 no.12
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    • pp.1781-1784
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    • 2003
  • Determination of Co(II) ion as a 4-(2-thiazolylazo)resorcinol(TAR) or 5-methyl-4-(2-thiazolylazo)resorcinol(5MTAR) chelate was accomplished by reversed-phase capillary high-performance liquid chromatography (RP-Capillary-HPLC) using a Vydac $C_4$ column and MeCN-water mixture as mobile phase. The effect of change in pH and MeCN percentage of the mobile phase on the retention factor, k and peak intensity were evaluated. It was found that 30% MeCN (v/v) of pH 5.60 or 7.20 was adequate as mobile phase when TAR or 5MTAR is used. Detection limit (D.L., S/N=3) in each case was $2.0\;{\times}\;10^{-7}$M (11.8 ppb) and $3.0\;{\times}\;10^{-7}$ M (17.7 ppb). The Co(II) ion in mineral and waste water was determined with the optimum column and mobile phase.

Electrode Surface Analysis of Delithiated $LiCoO_2$ using Ion Chromatograph (이온 크로마토그래피를 이용한 충전전압에 따른 $LiCoO_2$ 전극의 표면 특성)

  • Kim, Dong-Hun;Shin, Hye-Min;Chung, Young-Dong;Veluchamy, A.;Doh, Chil-Hoon;Jin, Bong-Soo;Moon, Seong-In;Kim, Hyun-Soo;Oh, Dae-Hui;Kim, Ki-Won
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2007.11a
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    • pp.498-499
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    • 2007
  • In this paper, we report on a study of the electrode/electrolyte interfaces of MCMB/$LiCoO_2$ cell using Ion-chromatography. The cells for the experiments were preconditioned by cycling three times and stabilized at OCV of 3.0V 4.35V and 4.5V. The stabilized cathode electrode was used for surface characterization investigations. Concerning the $LiCoO_2$/electrolyte interfaces, the result obtained have shown the presence of $F^-\;and\;CO_3^{2-}$ on the surface of cathode electrode as well as increasing the concentration of ions as cell voltage increase.

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Studies on the Toxic Activity of Bacillus sphaericus Spo -D1216 Asporogenic Mutant (Bacillus sphaericus Asporogenic Mutant Spo - D1216의 독성에 관한 연구)

  • 복거중;김영한;이형환
    • Microbiology and Biotechnology Letters
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    • v.13 no.2
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    • pp.157-162
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    • 1985
  • The cell cultures and crude extracts of Bacillus sphaericus 1593 K-5 and its mutant Spo-Dl216 were respectively bioassayed against Culex pipiens var. pollens mosquito larvae. The B. sphaeriucs 1593 K-5 showed toxic activity against the larvae. LC$_{50}$ values (cells/$m\ell$) was 2.6$\times$10$^2$. Also the LC$_{50}$ ($\mu\textrm{g}$ Protein/$m\ell$) of the crude extract was 10.26. However, B. sphaericus Spo-Dl216 didn't show toxic activity against the larvae. The soluble cytoplasmic toxin in broken B. sphaeriucs 1593k-5 cells was partially purified by gel permeation chromatography and ion exchange chromatography. Among the fractions of the gel permeation chromatography only a single fraction was found to be toxic. LC$_{50}$ values ($\mu\textrm{g}$ protein/$m\ell$) of the active fraction was 0.182. The active fraction of the gel permeation was subjected to ion exchange chromatography. Only a single fraction showed toxic activity and its LC$_{50}$ values ($\mu\textrm{g}$ protein/$m\ell$) was 0.02..02.

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Evaluation of measurement uncertainty for quantitative determination of chlorite and chlorate in fresh-cut vegetables using ion chromatography

  • Jung, Sungjin;Kim, Dasom;Lee, Gunyoung;Yun, Sang Soon;Lim, Ho Soo;Jung, Young Rim;Kim, Hekap
    • Korean Journal of Food Science and Technology
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    • v.49 no.6
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    • pp.591-598
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    • 2017
  • This study aimed to evaluate the measurement uncertainty for the quantitative determination of chlorite and chlorate in ready-to-eat fresh-cut vegetables using ion chromatography with a hydroxide-selective column. One gram of the homogenized sample in deionized water was sonicated and centrifuged at 8,500 rpm. The supernatant was purified by passing it through a Sep-Pak tC18 cartridge, followed by chromatographic determination using a Dionex IonPac AS27 column. The linearity of the calibration curves, recovery, repeatability, and reproducibility of the method were satisfactory. The method detection limit was estimated to be approximately 0.5 mg/kg. Each uncertainty component was evaluated separately, and the combined and expanded uncertainty values were calculated at the 95% confidence level. The measured concentrations for 3 mg/kg of chlorite and chlorate standard materials were $3.18{\pm}0.32$ and $3.10{\pm}0.42mg/kg$, respectively. These results confirmed the reliability of the developed method for measuring the two chlorine-based oxyanions in fresh-cut vegetables.

Identification of Fatty Acids in the Oils of Pine Nuts by GC-MS of Their Picolinyl Esters and 4,4-dimethyloxazoline Derivatives in Combination with Silver-Ion Chromatography

  • Kim, Seong-Jin;Woo, Hyo-Kyeng;Seo, Min-Young;Joh, Yong-Goe
    • Journal of the Korean Applied Science and Technology
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    • v.19 no.3
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    • pp.222-244
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    • 2002
  • A mixture of methyl ester derivatives of fatty acids from the oils of pine nuts was well resolved to five fractions differing by degree of unsaturation by silver ion solid-phase extraction column chromatography ($Ag^{+}$-SEC). Polyunsaturated fatty acid with non-methylene interrupted conjugated double bond (NMiDB) radical held more strongly to silver ions in the column than methylene interrupted conjugated double bond (MiDB) one when they had the same number of double bonds. Although both the picolinyl ester and DMOX derivative provided clear mass ion species powerful enough to elucidate the structure of the polyunsaturated fatty acid (PUFA) with NMiDB and/or methylene interrupted conjugated double bond (MiDB) radical in the oils, the picolinyl ester of PUFA with NMiDB radical did not provide a cluster of mass ions neighboring diagnostic mass ions induced by the double bond in the proximal to the carboxyl group. However, the DMOX derivative of PUFA with NMiDB group as well as MiDB showed abundant mass ion species differing by gaps of 12 amu, which made it possible with greater ease to locate the double bonds in the molecule. The oil contained $C_{18:2{\omega}6}$ (46.2 %) and $C_{18:1{\omega}9}$ (25.4 %) as main components, and considerable amounts of PUFAs with NMiDB radical such as ${\Delta}^{5.\;9.\;12}-C_{18:3}$ (16.0 %), ${\Delta}^{5.\;9}-C_{18:2}$ (2.3 %) and ${\Delta}^{5.\;11.\;14}-C_{20:3}$ (0.8 %).

Determination of Glimepiride in Human Plasma by Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

  • Kim, Ho-Hyun;Chang, Kyu-Young;Lee, Hee-Joo;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • v.25 no.1
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    • pp.109-114
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    • 2004
  • A sensitive method for quantitation of glimepiride in human plasma has been established using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Glipizide was used as an internal standard. Glimepiride and internal standard in plasma sample was extracted using diethyl etherethyl acetate (1 : 1). A centrifuged upper layer was then evaporated and reconstituted with the mobile phase of acetonitrile-5 mM ammonium acetate (60:40, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS in the multiple reaction monitoring (MRM) mode, glimepiride and glipizide were detected without severe interference from human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]$^+$) at m/z 491 and a corresponding product ion at m/z 352. And the internal standard produced a protonated precursor ion ([M+H]]$^+$) at m/z 446 and a corresponding product ion at m/z 321. Detection of glimepiride in human plasma by the LC-ESI/MS/MS method was accurate and precise with a quantitation limit of 0.1 ng/mL. The validation, reproducibility, stability, and recovery of the method were evaluated. The method has been successfully applied to pharmacokinetic studies of glimepiride in human plasma.

Isolation and Partial Characterization of Cysteine Proteinase from Sparganum (스파르가눔 총체에서 분리한 cysteine proteinase의 정제 및 부분 특성)

  • 송철용;최동호
    • Parasites, Hosts and Diseases
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    • v.30 no.3
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    • pp.191-200
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    • 1992
  • A proteolytic enzyme was purified from the tissue extract of spargana (plerocercoids of Spirometra erinacei) by DEAE-Trisacryl M ion exchange chromatography and thiopropyl-sepharose affinity chromatography resulted in a 21-fold purification. The proteinase activity was assayed with a synthetic fluorescent substrate, carbobensoxy-phenylalanyl-7-amiso-4-trifluoromethyl-coumarin. SDS-polyacplamide gel electrophoresis of the purified materials revealed a single 28,000 dalton band. Inhibitor profiles of the band indicated that it belonged to cysteine endopeptidases. It exhibited identical pH curves with optimum at pH 5,5, and 50% activity from pH 4.7 to 8. It could completely degrade collagen chains to three identical products. It also showed some activity on hemoglobin. Furthermore, the band on immunoblots was reactive to the sera of sparganosis patients. These results suggest that the proteolytic enzyme belongs to cysteine proteinase which plays a role in the tissue penetration. Also it may be used as the antigen for diagnosis of active sparganosis.

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