• Title/Summary/Keyword: ion-pair

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Characterization of the Fragmentation Pattern of Peptide from Tandem Mass Spectra

  • Ramachandran, Sangeetha;Thomas, Tessamma
    • Mass Spectrometry Letters
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    • v.10 no.2
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    • pp.50-55
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    • 2019
  • The fragmentation statistics of ion trap CID (Collision-Induced Dissociation) spectra using 87,661 tandem mass spectra of doubly charged tryptic peptides are analyzed here. In contrast to the usual method of using intensity information, the frequency of occurrence of fragment ions, with respect to the position of the cleavage site and the residues at these sites is studied in this paper. The analysis shows that the frequency of occurrence of fragment ion peaks is more towards the middle of the peptide than its ends. It was noted that amino acid with an aromatic and basic side chain at N- & C- terminal end of the peptide stimulates more peaks at the lower end of the spectrum. The residue pair effect was shown when the amide bond occurs between acidic and basic residues. The fragmentation at these sites (D/E-H/R/K) stimulates the generation of the y-ion peak. Also, the cleavage site H-H/R/K stimulates the generation of b-ions. K-P environment in the peptide sequence has more tendency to generate y-ions than b-ions. Statistical analysis helps in the visualization of the CID fragmentation pattern. Cleavage pattern along the length of the peptide and the residue pair effects, enhance the knowledge of fragmentation behavior, which is useful for the better interpretation of tandem mass spectra.

Separation and Determination of Acteoside in Pedicularis resupinata var. oppositifolia by Ion Pair Liquid Chromatography (이온쌍 액체 크로마토그래피에 의한 마주송이풀 중의 Acteoside의 분리와 정량)

  • Yun, Young Ja;Yu, Gu Yong
    • Analytical Science and Technology
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    • v.8 no.2
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    • pp.161-166
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    • 1995
  • Determination of acteoside in Pedicularis resupinata var. oppositifolia has been studied using ion pair liquid chromatography. Sample was extracted with 40mL methanol for 4 hrs. The extract was cleaned up by using Sep-Pak $C_{18}$ catridge and 8mL aqueous methanol eluent(methanol 50%, water 50%, phosphate buffer pH=8.0). Its determination was performed by means of IP-HPLC with a Hamilton PRP-1 polystyrene-divinylbenzene reversed phase column($15cm{\times}4.6mm$ i. d., $5{\mu}m$) and an aqueous methanol eluent(methanol 60%, water 40% phosphate buffer pH=8.2) containing of $5.0{\times}10^{-3}M$ tetrabutylammonium bromide. The established method was applied to the sample that was collected in area of Pyung Chang gun. As a result, its content ranges showed to be 0.062~0.076%.

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Determination of Boron by Ion Pair Liquid Chromatography with Chromotropic Acid (Chromotropic Acid를 착화제로 이용한 이온쌍 액체 크로마토그래피에 의한 붕소의 분리와 정량)

  • Yun, Young Ja;Yu, Gu Yong
    • Journal of the Korean Chemical Society
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    • v.39 no.4
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    • pp.288-293
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    • 1995
  • The separation and determination of boron with chromotropic acid (1,8-Dihydroxynaphthalene-3,6-disulfonic acid) as a complex agent has been studied using ion pair liquid chromatography. The use of tetrabutylammonium bromide added as an ion pair reagent to mobile phase (MeOH 61%, phosphate buffer 39% pH=8.5) allowed good separation of boron-chromotrophic acid complex anion and chromotrophic acid on poly(styrene-divinylbenzene) based reversed phase column (PRP-1, 15 $cm{\times}4.6$ mm i.d.). The complex formation between boric acid and chromotrophic acid was enhanced in the presence of 0.1 M tetrabutylammonium bromide, resulting in high sensitivity. The linear calibration was achieved over the boron concentration range of 0.5∼1000 ${\mu}g/L.$ The detection limit was 0.5 ${\mu}g/L$ (S/N=2). The proposed method was applied to the determination of boron in commercially available chemicals, $Na_2SO_4$, NaOH, KCl.

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Altered Pharmacokinetics and Hepatic Uptake of TBuMA in Ethynylestradio-Induced Cholestasis

  • Hong Soon-Sun;Choi Jong-Moon;Jin Hyo-Eon;Shim Chang-Koo
    • Archives of Pharmacal Research
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    • v.29 no.4
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    • pp.323-327
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    • 2006
  • The objective of this study was to examine the pharmacokinetics of organic cations in intrahepatic cholestatic rats. A pretreatment with $17{\alpha}$-ethynylestradiol was used to induce intrahepatic cholestasis, and tributylmethylammonium (TBuMA) was used as a representative model organic cation. When $[^3H]$TBuMA was intravenously administered, the AUC value for TBuMA was significantly increased by $79\%$ in cholestasis, and its total systemic clearance was consequently decreased by $46\%$. In addition, the in vivo hepatic uptake clearance of TBuMA from the plasma to the liver was decreased by $50\%$ in cholestasis. The concentration of bile salts in plasma was increased by 2.1 fold in cholestatic rats. Since TBuMA forms ion-pair complexes with anionic components such as bile salts, the decreased hepatic uptake of TBuMA in cholestasis may be due to a change in endogenous components, e.g., bile salts in the plasma. In isolated normal hepatocytes, the uptake clearance for TBuMA in the presence of cholestatic plasma was decreased by $20\%$ compared with normal plasma. Therefore, we conclude that the inhibition of the hepatic uptake process by the cholestasis may be in part due to the increased formation of ion-pair complexes of TBuMA with bile salts in the plasma.

Determination of Trace Mo(VI) in Seawater Samples by Ion Pair Formation and Solvent Extraction (이온쌍 형성-용매추출에 의한 해수 중 극미량 Mo(VI)의 정량)

  • Kim, Young-Sang;Nho, Seung-Gu;Choi, Jong-Moon
    • Analytical Science and Technology
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    • v.6 no.3
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    • pp.329-334
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    • 1993
  • The formation of Mo(VI)-alizarin red S chelate ion its extraction into an organic solvent by ion-pairing for the separarive determination of trace Mo(VI) in natural water was applied in seawater samples. Removed Fe(III) and Zn(II), and Cu(II) by precipitating with anthranilic acid at pH 4.0 and 2.0, seawater 100mL was sampled in 250mL separatory funnel. After Mo(VI)-ARS chelate ion was formed by adding 0.01M alizarin red S solution 1.0mL to the water sample of pH 4.6, 0.6% aliquat-336 chloroform solution 10mL was added and the solution was vigorously shaked for about 30 seconds to form the ion-pair between Mo(VI)-ARS and aliquat-336 perfectly. The solution was stood for about 30 minutes. And the organic phase was taken for the absorbance measurement of the ion-pair at 520nm. The content of Mo(VI) was obtained from the standard calibration curve. Several extraction conditions such as pH, adding amounts of alizarin red S and aliquat-336, and shaking and standing times were optimized and the interferences and release of concomitant ions was also studied. This procedure was applied to the analysis of Eastern and Yellow seawaters. It could be confirmed from the recoveries of over 85% in samples spiked with a given amount of Mo(VI) that this method was also quantitative in the determination of trace Mo(VI) in a seawater.

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Effect of Ion Pair on Thermostability of F1 Protease: Integration of Computational and Experimental Approaches

  • Rahman, Raja Noor Zaliha Raja Abd;Noor, Noor Dina Muhd;Ibrahim, Noor Azlina;Salleh, Abu Bakar;Basri, Mahiran
    • Journal of Microbiology and Biotechnology
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    • v.22 no.1
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    • pp.34-45
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    • 2012
  • A thermophilic Bacillus stearothermophilus F1 produces an extremely thermostable serine protease. The F1 protease sequence was used to predict its three-dimensional (3D) structure to provide better insights into the relationship between the protein structure and biological function and to identify opportunities for protein engineering. The final model was evaluated to ensure its accuracy using three independent methods: Procheck, Verify3D, and Errat. The predicted 3D structure of F1 protease was compared with the crystal structure of serine proteases from mesophilic bacteria and archaea, and led to the identification of features that were related to protein stabilization. Higher thermostability correlated with an increased number of residues that were involved in ion pairs or networks of ion pairs. Therefore, the mutants W200R and D58S were designed using site-directed mutagenesis to investigate F1 protease stability. The effects of addition and disruption of ion pair networks on the activity and various stabilities of mutant F1 proteases were compared with those of the wild-type F1 protease.

Continuous ion-exchange membrane electrodialysis of mother liquid discharged from a salt-manufacturing plant and transport of Cl- ions and SO42- ions

  • Tanaka, Yoshinobu;Uchino, Hazime;Murakami, Masayoshi
    • Membrane and Water Treatment
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    • v.3 no.1
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    • pp.63-76
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    • 2012
  • Mother liquid discharged from a salt-manufacturing plant was electrodialyzed at 25 and $40^{\circ}C$ in a continuous process integrated with $SO_4{^{2-}}$ ion low-permeable anion-exchange membranes to remove $Na_2SO_4$ and recover NaCl in the mother liquid. Performance of electrodialysis was evaluated by measuring ion concentration in a concentrated solution, permselectivity coefficient of $SO_4{^{2-}}$ ions against $Cl^-$ ions, current efficiency, cell voltage, energy consumption to obtain one ton of NaCl and membrane pair characteristics. The permselectivity coefficient of $SO_4{^{2-}}$ ions against $Cl^-$ ions was low enough particularly at $40^{\circ}C$ and $SO_4{^{2-}}$ transport across anion-exchange membranes was prevented successfully. Applying the overall mass transport equation, $Cl^-$ ion and $SO_4{^{2-}}$ ion transport across anion-exchange membranes is evaluated. $SO_4{^{2-}}$ ion transport number is decreased due to the decrease of electro-migration of $SO_4{^{2-}}$ ions across the anion-exchange membranes. $SO_4{^{2-}}$ ion concentration in desalting cells becomes higher than that in concentration cells and $SO_4{^{2-}}$ ion diffusion is accelerated across the anion-exchange membranes from desalting cells toward concentrating cells.

이온토포레시스에 의한 극성약물의 경피흡수 촉진

  • 심창구;김종국
    • Proceedings of the Korean Society of Applied Pharmacology
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    • 1992.05a
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    • pp.62-62
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    • 1992
  • 1.이온토포레시스에 의한 ISP의 경피촙수증가는 단순투과의 약 13배로서 그 증가정도는 전류세기와 약물농도에 비례하였다. 2. 가해주는 $Na^{+}$ 농도가 커질수록 ISP의 flux는 감소하였다. 3. ion-pairing agent률 가하면 ISP의 flux는 감소하는데, 그 감소정도는 TU>SAL>BEN 로서 이는 이 물질들이 ISP와 ion-pair를 형성하는 능력순서와 같았다. 4. ISP용액의 pH증가시 ISP의 flux는 대체적으로 증가하며 그 pattern은 피부의 pKa를 3.5로 가정할 때의 피부해리곡선과 유사하였다. ISP가 광범위한 pH에서 완벽하게 해리된다고 가정할 때 pH증가시 flux증가는 피부해리 증가에 따른 permselectivity 증가에 기인한 것으로 생각되었다.

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Fast Protein Staining in Sodium Dodecyl Sulfate Polyacrylamide Gel using Counter ion-Dyes, Coomassie Brilliant Blue R-250 and Neutral Red

  • Choi, Jung-Kap;Yoo, Gyurng-Soo
    • Archives of Pharmacal Research
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    • v.25 no.5
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    • pp.704-708
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    • 2002
  • A fast and sensitive protein staining method in sodium dodecyl sulfate-polyacrylamide gel electrophoresis (SDS-PAGE) using both an acidic dye, Coomassie Brilliant Blue R-250 (CBBR) and a basic dye, Neutral Red (NR) is described. It is based on a counter ion-dye staining technique that employs oppositely charged two dyes to form an ion-pair complex. The selective binding of the free dye molecules to proteins in an acidic solution enhances the staining effect of CBBR on protein bands, and also reduces gel background. It is a rapid staining procedure, involving fixing and staining steps with short destaining that are completed in about 1 h. As the result, it showed two to fourfold increase in sensitivity comparing with CBBR staining. The stained protein bands can be visualized at the same time of staining.

Chromatographic Separation of Lithum Isotopes by Hydrous Managanese(Ⅳ) Oxide (가수된 산화 망간(Ⅳ)에 의한 리튬 동위원소의 크로마토그래피적 분리)

  • Kim, Dong Won
    • Journal of the Korean Chemical Society
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    • v.45 no.3
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    • pp.219-222
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    • 2001
  • Separation of lithium isotopes was investigated by chemical ion exchange with a hydrous manganese(IV) oxide ion exchanger using an elution chromatography. The capacity of manganese(IV) oxide ion exchanger was 0.5 meq/g. The heavier lithium isotope was enriched in the solution phase, while the lighter isotope was enriched in the ion exchanger phase. The separation factor was determined according to the method of Glueckauf from the elution curve and isotopic assays. The separation factor of $^6Li^+$-$^7Li^+$ isotope pair fractionation was 1.018.

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