• Title/Summary/Keyword: Weak anion-exchange

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A Multidimensional System for Phosphopeptide Analysis Using TiO2 Enrichment and Ion-exchange Chromatography with Mass Spectrometry

  • Cho, Kun;Yoo, Ji-Sun;Kim, Eun-Min;Kim, Jin-Young;Kim, Young-Hwan;Oh, Han-Bin;Yoo, Jong-Shin
    • Bulletin of the Korean Chemical Society
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    • v.33 no.10
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    • pp.3298-3302
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    • 2012
  • Although offline enrichment of phosphorylated peptides is widely used, enrichment for phosphopeptides using $TiO_2$ is often performed manually, which is labor-intensive and can lead to irreproducible results. To address the problems associated with offline enrichment and to improve the effectiveness of phosphopeptide detection, we developed an automated online enrichment system for phosphopeptide analysis. A standard protein mixture comprising BSA, fetuin, crystalline, ${\alpha}$-casein and ${\beta}$-casein, and ovalbumin was assessed using our new system. Our multidimensional system has four main parts: a sample pump, a 20-mm $TiO_2$-based column, a weak anion-exchange, and a strong cation-exchange (2:1 WAX:SCX) separation column with LC/MS. Phosphorylated peptides were successfully detected using the $TiO_2$-based online system with little interference from nonphosphorylated peptides. Our results confirmed that our online enrichment system is a simple and efficient method for detecting phosphorylated peptides.

Modeling the electric transport of HCl and H3PO4 mixture through anion-exchange membranes

  • Koter, Stanislaw;Kultys, Monika;Gilewicz-Lukasik, Barbara
    • Membrane and Water Treatment
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    • v.2 no.3
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    • pp.187-205
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    • 2011
  • The electric transport of the mixture of hydrochloric and phosphoric acids through strong base (Neosepta ACM) and weak base (Selemion AAV) anion-exchange membranes was investigated. The instantaneous efficiency of HCl removal from the cathode solution, $CE_{Cl}$, with and without $H_3PO_4$ was determined. It was found that $CE_{Cl}$ was 0.8-0.9 if the number of moles of elementary charge passed through the system, $n_F$, did not exceed ca. 80% of the initial number of HCl moles in the cathode solution, $n_{Cl,ca,0}$. The retention efficiency of $H_3PO_4$ in that range was close to one. The transport of acid mixtures was satisfactorily described by a model based on the extended Nernst-Planck and Donnan equations for $n_F$ not exceeding $n_{Cl,ca,0}$. Among the tested model parameters, most important were: concentration of fixed charges, the porosity-tortuosity coefficient, and the partition coefficient of an undissociated form of $H_3PO_4$. For the both membranes, the obtained optimal values of fixed charge concentration, $\bar{c}_m$, were up to 40% lower than the literature values of $\bar{c}_m$ obtained from the equilibrium measurements. Regarding the $H_3PO_4$ equilibria, it was sufficient to consider $H_3PO_4$ as a monoprotic acid.

Enantioseparation of Neutral Compounds on a Quinine Carbamate-Immobilized Zirconia in Reversed-Phase Capillary Electrochromatography

  • Lee, Mun-Rak;Gwon, Ju-Rim;Park, Jung-Hag
    • Bulletin of the Korean Chemical Society
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    • v.31 no.1
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    • pp.82-86
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    • 2010
  • Quinine (QN) is a weak anion-exchange type chiral selector and QN-based silica stationary phases have been widely used for enantioseparation of acidic chiral analytes in HPLC and recently in CEC. In this work we report enantioseparation of non-acidic chiral analytes on a quinine carbamate-immobilized zirconia (QNZ) in reversed-phase (RP) CEC. Influences of pH, composition of the buffer, acetonitrile content and the applied voltage on enantioseparation were examined. Enantiomers of the analytes investigated are well separated in acetonitrile/phosphate buffer mobile phases. Separation data on QNZ were compared to those on QN-bonded silica (QNS). Retention was longer but better enantioselectivity and resolution were obtained on QNZ than QNS.

Influence of Jahn-Teller Distortion on the Magnetic Coupling in Oxalato-Bridged Copper(II) Dimers: An Orbital Interpretation of the Superexchange Mechanism

  • Kang, Dae-Bok
    • Bulletin of the Korean Chemical Society
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    • v.26 no.12
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    • pp.1965-1968
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    • 2005
  • Extended H$\ddot{u}$ckel molecular calculations have been used to analyze how the magnitude of exchange coupling is influenced by the structural distortions in a series of dinuclear six-coordinate copper(II) complexes bridged by the planar bis-bidentate oxalate anion. Copper(II) ions have distorted octahedral surroundings, one being axially elongated and the other compressed. The magnetic interaction is strong in the former complexes and very weak in the latter. This is interpreted as resulting from a switching of magnetic spin orbitals due to the structural distortions (bond elongation or compression) of the copper sites.

Peptide Profiling and Selection of Specific-Expressed Peptides in Hypoglycemic Sorghum Seed using SELDI-TOF MS (SELDI-TOF MS를 활용한 혈당강하 수수 종자의 펩타이드 프로파일링 및 특이 발현 펩타이드 선발)

  • Park, Sei Joon;Hwang, Su Min;Park, Jun Young;Ko, Jee-Yeon;Kim, Tae Wan
    • KOREAN JOURNAL OF CROP SCIENCE
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    • v.59 no.3
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    • pp.252-262
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    • 2014
  • Sorghum seed is traditionally used as secondary food sources in addition to rice in Korea. While the hypoglycemia regulating phytochemicals have been found in sorghum seed, peptides related with hypoglycemia never been studied before. To obtain the peptide characteristics and the specifically high-expressed peptides in hypoglycemic sorghum seed, peptide profiles of seven hypoglycemic and five non-hypoglycemic sorghum lines bred in RDA were determined using surface-enhanced laser desorption/ionization time-of-flight mass spectrometry (SELDI-TOF MS). The twelve sorghum lines exhibited 104 peptides on CM10 protein chip array (weak cation exchange) and 95 peptides on Q10 (weak cation exchange) in the molecular mass range from 2,000 to 20,000 Da. Heat map via supervised hierarchical clustering of the significantly different peptides (p < 0.01) in peak intensity among the 12 lines effectively revealed the specifically upregulated peptides in each line and distinguished between 7 hypoglycemic and 5 non-hypoglycemic lines. Through the comparison with hypoglycemic and non-hypoglycemic lines, 10 peptides including 2231.6, 2845.4, 2907.9, 3063.5, 3132.6, 3520.8, 4078.8, 5066.2, 5296.5, 5375.5 Da were specifically high-expressed in hypoglycemic lines at p < 0.00001. This study characterized seed peptides of 12 sorghums and found ten peptides highly expressed for hypoglycemic sorghum lines, which could be used as peptide biomarkers for identification of hypoglycemic sorghum.

Crystal Structures and Magnetic Properties of Sparteinium Tetrahalocuprate Monohydrate Compounds

  • Lee, Yong-Min;Park, Sung-Min;Kang, Sung-Kwon;Kim, Young-Inn;Choi, Sung-Nak
    • Bulletin of the Korean Chemical Society
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    • v.25 no.6
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    • pp.823-828
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    • 2004
  • The crystal structures of sparteinium tetrachlorocuprate monohydrate $[(C_{15}H_{28}N_2)CuCl_4{\cdot}H_2O]$, 1 and sparteinium tetrabromocuprate monohydrate $[(C_{15}H_{28}N_2)CBr_4{\cdot}H_2O]$, 2, were determined. The structures of 1 [orthorhombic, $P2_12_12_1$, a = 8.3080(10) ${\AA}$, b = 14.6797(19) ${\AA}$ and c = 16.4731(17) ${\AA}$], and 2 [orthorhombic, $P2_12_12_1$, a = 8.4769(7) ${\AA}$, b = 15.166(3) ${\AA}$ and c = 16.679(3) ${\AA}$], are composed of a doubly protonated sparteinium cation, $[C_{15}H_{28}N_2]^{2+}$, a discrete $CuX_4^{2-}$ anion $(X=Cl^-\;or\;Br^-)$, and one water molecule. These monomeric compounds are stabilized through various types of hydrogen bonding interaction in their packing structures. Crystal 2 exhibits weak anti-ferromagnetism (J = -3.24 $cm^{-1}$) as opposed to the magnetically isolated paramagnetism observed for 1. The results of comparative magneto-structural investigations of 1 and 2 suggest that the pathway for the weak anti-ferromagnetic super-exchange in 2 might be through a Cu-Br${\cdots}$Br-Cu contact.

Anticancer Activity of Sulfated Polysaccharides Isolated from the Antarctic Red Seaweed Iridaea cordata

  • Kim, Hak Jun;Kim, Woo Jung;Koo, Bon-Won;Kim, Dong-Woo;Lee, Jun Hyuck;Nugroho, Wahyu Sri Kunto
    • Ocean and Polar Research
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    • v.38 no.2
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    • pp.129-137
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    • 2016
  • This study aimed to isolate and characterize sulfated polysaccharides (SPs) from Iridaea cordata and evaluate their anticancer activity. SPs of the Antarctic red seaweed were obtained by $CaCl_2$ (SP1) and ethanol precipitations (SP2) following diluted acid extraction at room temperature. Yields of SP1 and SP2 were approximately 14% and 23%, respectively, of the dry weight of red seaweed. The average molecular mass of the SP1 and SP2 was estimated about $1.84{\times}10^3$ and $1.42{\times}10^3kDa$, respectively, by size-fractionation High-Performance Liquid Chromatography (HPLC). From the High-Performance Anion-Exchange Chromatography-Pulsed Amperometric Detection (HPAEC-PAD) analysis, the main monosaccharide was galactose with glucose and fucose as minor components. The sulfate content of SP2 (40.4%) was slightly higher than that of SP1 (33.8%). The FT-IR spectra also showed characteristic band of carrageenan-like sulfated polysaccharides. Taken together the SPs are thought to be carrageenan-like sulfated galactan. The polysaccharides (SPs) from I. cordata exhibited weak antitumor activity against PC-3 (prostate cancer), HeLa (cervical cancer), and HT-29 (human colon adenocarcinoma). To our knowledge, this is the first data on biological activity of the Antarctic red seaweed I. cordata.

Purification and Characterization of an Acid Deoxyribonuclease from the Cultured Mycelia of Cordyceps sinensis

  • Ye, Maoqing;Hu, Zheng;Fan, Ying;He, Ling;Xia, Fubao;Zou, Guolin
    • BMB Reports
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    • v.37 no.4
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    • pp.466-473
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    • 2004
  • A new acid deoxyribonuclease (DNase) was purified from the cultured mycelia of Cordyceps sinensis, and designated CSDNase. CSDNase was purified by $(NH_4)_2SO_4$ precipitation, Sephacryl S-100 HR gel filtration, weak anion-exchange HPLC, and gel filtration HPLC. The protein was single-chained, with an apparent molecular mass of ca. 34 kDa, as revealed by SDS-PAGE, and an isoelectric point of 7.05, as estimated by isoelectric focusing. CSDNase acted on both double-stranded (ds) and single- stranded (ss) DNA, but preferentially on dsDNA. The optimum pH of CSDNase was pH 5.5 and its optimum temperature 55. The activity of CSDNase was not dependent on divalent cations, but its enzymic activity was inhibited by high concentration of the cation: $MgCl_2$ above 150 mM, $MnCl_2$ above 200 mM, $ZnCl_2$ above 150 mM, $CaCl_2$ above 200 mM, NaCl above 300 mM, and KCl above 300 mM. CSDNase was found to hydrolyze DNA, and to generate 3-phosphate and 5-OH termini. These results indicate that the nucleolytic properties of CSDNase are essentially the same as those of other well-characterized acid DNases, and that CSDNase is a member of the acid DNase family. To our knowledge, this is the first report of an acid DNase in a fungus.

Distribution of PFOA and PFOS in Maternal Blood, Cord Blood and Breast Milk in Busan (부산 지역 임산부의 모체혈, 제대혈, 모유에서 PFOA, PFOS의 농도)

  • Suh, Chun-Hui;Lee, Chae-Kwan;Kim, Kun-Hyung;Son, Byung-Chul;Lee, Jong-Tae
    • Journal of Environmental Health Sciences
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    • v.38 no.1
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    • pp.8-17
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    • 2012
  • Objectives: Perfluorooctanoic acid (PFOA) and perfluorooctane sulfonate (PFOS) are man-made, persistent global pollutants widely diffused throughout the environment. They have been even found in the cord blood and breast milk of humans. Furthermore evidence of developmental toxicity in animals exists. To assess the distribution of maternal and fetal exposure to PFOS and PFOA, we analyzed paired maternal blood, cord blood and breast milk samples. Methods: Maternal blood, cord blood and breast milk were collected from 150 volunteers from the general population (aged 20-40, mean $30.5{\pm}2.9$) of the city of Busan in 2009-2010. The samples were extracted using the weak anion exchange and solid-phase extraction methods and quantified by high-performance liquid chromatograph (HPLC, Agilent 1200 Series) coupled with an Triple Quad LC-MS/MS system (Agilent 6410). Results: Median PFOA and PFOS concentrations in maternal blood were 2.18 and 3.32 ng/ml, in cord blood were 0.83 and 0.58 ng/ml, and in breast milk were 0.13 and 0.11 ng/ml, respectively. PFOS and PFOA concentrations were significantly correlated among matrices (Spearson's ${\rho}=0.226$, p = 0.05 for maternal blood; ${\rho}=0.736$, p < 0.01 for cord blood; ${\rho}=0.493$ p < 0.01 for breast milk). The ratio of cord blood/maternal blood was 0.39 for PFOA and 0.19 for PFOS. The ratio of breast milk/maternal blood was 0.07 for PFOA and 0.06 for PFOS. Conclusions: Our findings suggest that PFOA and PFOS exposure through the placenta was more prominent than through breast milk among Korean neonates born in Busan. The transfer efficiency of maternal blood to breast milk was similar between PFOA and PFOS, but that of maternal blood to cord blood was higher in PFOA than PFOS.