• Title/Summary/Keyword: H-NMR spectroscopy

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Synthesis and Analytical Application of Piperidine Dithiocarbamate Complex of Copper(II) (피페리딘 디티오카바메이트의 구리(II)의 착물합성과 분석적 응용)

  • Kim, Chan-Woo;Kim, Chang-Su
    • Analytical Science and Technology
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    • v.12 no.1
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    • pp.1-6
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    • 1999
  • Copper(II) complex of piperidine dithiocarbamate (Pipdtc) was synthesized from the reaction of Cu(II) and piperidine dithiocarbamate. The possible structure of the complex was proposed on the basis of elemental analysis, molar conductivity, infrared spectroscopy, electronic absorption spectroscopy, and $^{13}C-NMR$ studies. The extraction of copper(II)-Pipdtc complex by carbon tetrachloride can be achieved in the pH range of 6.0~10. The solution of copper(II) with piperidine dithiocarbamate was bey Beer's law in the concentration up to ${\sim}8.0{\times}10^{-5}M$ at pH 9.0.

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Comparison of Physicochemical Properties between Ursodeoxycholic Acid and Chenodeoxycholic Acid Inclusion Complexes with ${\beta}-Cyclodextrin$ (우르소데옥시콜린산 및 케노데옥시콜린산의 베타시클로덱스트린 포접복합체의 물리화학적 특성비교)

  • Lee, Seung-Yong;Chung, Youn-Bok;Han, Kun;Shin, Jae-Young
    • YAKHAK HOEJI
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    • v.38 no.3
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    • pp.300-310
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    • 1994
  • Physicochemical properties for the inclusion complex of chenodeoxycholic acid(CDCA) and it's $7{\beta}-hydroxy$ epimer ursodeoxycholic acid(UDCA) with ${\beta}-cyclodextrin({\beta}-CyD)$ were studied. The formation of the complex in the solid state were confimed by polarized microscopy and differential scanning calorimetry(DSC). Proton nuclear magnetic resonance$(^1H-NMR)$spectroscopy showed that CDCA and UDCA form an inclusion complex with ${\beta}-CyD$ in aqueous solution. The 1 : 1 stoichiometry of the complex was dextermined by the continuous variation method. From DSC and $^1H-NMR$ studies, there were not any differences between CDCA and UDCA. Complex of CDCA and UDCA showed increase in solubility and dissolution compared with CDCA and UDCA alone, respectively. Solubility pattern of UDCA complex was pH independent but, CDCA complex was like that of CDCA. Dissolution rate increased markedly in case of UDCA complex compared with CDCA complex, especially in acidic pH value.

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Kinetic Study of Xylan Hydrolysis and Decomposition in Concentrated Sulfuric Acid Hydrolysis Process by $^1H$-NMR Spectroscopy ($^1H$-NMR에 의한 Xylan의 황산가수분해 과정에서 나타나는 반응 동력학 연구)

  • Cho, Dae-Haeng;Kim, Yong-Hwan;Kim, Byung-Ro;Park, Jong-Moon;Sung, Yong-Joo;Shin, Soo-Jeong
    • Journal of Korea Technical Association of The Pulp and Paper Industry
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    • v.43 no.3
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    • pp.52-58
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    • 2011
  • Proton-NMR spectroscopic method was applied to kinetic study of concentrated sulfuric acid hydrolysis reaction, especially focused on 2nd step of acid hydrolysis with deferent reaction time and temperature as main variables. Commercial xylan extracted from beech wood was used as model compound. In concentrated acid hydrolysis, xylan was converted to xylose, which is unstable in 2nd hydrolysis condition, which decomposed to furfural or other reaction products. Without neutralization steps, proton-NMR spectroscopic analysis method was valid for analysis of not only monosaccharide (xylose) but also other reaction products (furfural and formic acid) in acid hydrolyzates from concentrated acid hydrolysis of xylan, which was the main advantages of this analytical method. Higher temperature and longer reaction time at 2nd step acid hydrolysis led to less xylose concentration in xylan acid hydrolyzate, especially at $120^{\circ}C$ and 120 min, which meant hydrolyzed xylose was converted to furfural or other reaction products. Loss of xylose was not match with furfural formation, which meant part of furfural was degraded to other undetected compounds. Formation of formic acid was unexpected from acidic dehydration of pentose, which might come from the glucuronic acid at the side chain of xylan.

Chemical Structure Analysis of Non-ionic Monomer Contrast Agents Using 1H-NMR Spectroscopy (1H-NMR Spectroscopy를 이용한 Non-ionic Monomer 조영제의 화학적 구조 분석)

  • Han, Beom-Hee
    • Journal of radiological science and technology
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    • v.44 no.4
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    • pp.335-342
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    • 2021
  • Studies on the side effects of contrast agents are being discussed based on various cases, but studies analyzing the chemical structure of the underlying contrast agents are difficult to understand as the manufacturers have not disclosed them. Therefore, in this study, the chemical structure of the contrast medium was analyzed using 1H-NMR spectrometer for Omnipaque contrast medium prepared from Iohexol, which is a nonionic iodide contrast medium, Xenetix contrast medium from Iobitridol, and Iomeron contrast medium from Iomeprol. As a result, it was found that the Omnipaque contrast medium of Iohexol had 6 carboxyl groups, 3 carbonyl groups, 4 amine groups, 1 methyl group, and 2 cyano groups. It was found that the Xenetix contrast medium of the iobitridol formulation had 6 carboxyl groups, 3 carbonyl groups, 2 amine groups, and 4 cyano groups. It was found that the Iomeron contrast agent of the Iomeprol formulation had 5 carboxyl groups, 3 carbonyl groups, 4 amine groups, 1 methyl group, and 2 cyano groups. As shown in this study, the chemical structure of the non-ionic monomer contrast agent increases its affinity with water by binding a number of hydroxyl groups (OH) to the carboxyl group. It is necessary to accurately identify each of these factors and analyze the physical and chemical changes of the contrast medium according to various environmental factors.

NMR Studies of Metal-binding Luteinizing Hormone Releasing Hormone

  • Won, Ho-Shik
    • Bulletin of the Korean Chemical Society
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    • v.32 no.11
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    • pp.4021-4026
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    • 2011
  • Functions of the luteinizing hormone releasing hormone (LHRH) and its induced release by divalent metal ions have received great attention because this neurotransmitter subsequently regulates the secretion of luteinizing hormone (LH). Metal-LHRH complexes were synthesized by addition of various Cu(II),Ni(II),Zn(II) ions into LHRH in order to understand how the induced release of LHRH is possible. The degree of complexation was monitored by $^1H$, $^{13}C$-NMR chemical shifts, and final products were identified by Mass spectrometry. Solutionstate structure determination of Zn(II)-LHRH out of metal-complexes was accomplished by using NMR and NMR-based distance geometry (DG). Interproton distance information from nuclear Overhauser effect spectroscopy was utilized for structure determination. Structure obtained in this study has a cyclic conformation exhibiting a specific ${\alpha}$-helical turn with residue numbers His[2]-Leu[7] out of 10 amino acids. Comparison of chemical shifts and EPR studies of Ni(II),Cu(II)-LHRH complexes exhibit that these metal complexes have 4-coordination geometry.

Use of Nuclear Magnetic Resonance Spectroscopy in Analysis of Fennel Essential Oil

  • AbouZid, Sameh
    • Natural Product Sciences
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    • v.22 no.1
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    • pp.30-34
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    • 2016
  • A simple and rapid method based on proton nuclear magnetic resonance spectroscopy was developed for determination of trans-anethole content in fennel essential oil. Spectra of pure trans-anethole, of the pure essential oil of fennel, and of the pure oil of fennel with thymol internal standard were recorded. The signal of $H-1^/$ was used for quantification of trans-anethole. This proton signal is well separated in the proton magnetic resonance spectrum of the compound. No reference compound is needed and cheap internal standard was used. The results obtained from spectroscopic analysis were compared with those obtained by gas chromatography. Additionally, the developed method was used for determination of the type of vegetable oil used as a carrier in commercial products, which cannot be quantified as such by gas chromatography. This study demonstrates the application of proton nuclear magnetic resonance spectroscopy as a quality control method for estimation of essential oil components.

Establishment of a Simple and Rapid Method for Quantitative Determination of -Aminobutyric Acid Using 1H NMR and Production of γ-Aminobutyric Acid in Cell Suspension Cultures of Coriandrum sativum L. (1H NMR에 의한 γ-Aminobutyric Acid의 간단하고 신속한 정량분석법 확립과 고수 (Coriandrum sativum L.) 현탁배양세포로부터 γ-Aminobutyric Acid의 생산)

  • Kim, Suk-Weon;Liu, Jang-R.
    • Journal of Plant Biotechnology
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    • v.34 no.3
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    • pp.207-212
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    • 2007
  • This study describes a simple and rapid method for quantitative determination of $\gamma$-aminobutyric acid (GABA) using $^1H$ NMR spectroscopy from whole cell extracts of plant suspension cultures. When 9 cell lines derived from 8 species of higher plants maintained in liquid Marashige and Skoog (MS) medium supplemented with 1 mg/L 2,4-dichlorophenoxyacetic acid (2,4-D) were subjected to $^1H$ NMR, a cell line of Coriandrum sativum L. exhibited the highest level of GABA. The level reached up to 16.9 mg/dry wt when cells were cultured in MS medium supplemented with 0.5 mg/L 2,4-D after 3 weeks of incubation. The method for quantitative determination of GABA using $^1H$ NMR established in this study could be applied to high-throughput screening of various plant resources for GABA production and the cell suspension culture system of C. sativum could be further developed for commercial production of GABA.

Structure Study of Inclusion Complex of ${\beta}-Cyclodextrin$ and Aspirin (${\beta}$-시클로덱스트린과 아스피린의 포접화합물의 구조에 관한 연구)

  • Choi, Hee-Sook
    • Journal of Pharmaceutical Investigation
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    • v.21 no.4
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    • pp.223-230
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    • 1991
  • The structural specificity and the chemical dynamics between ${\beta}-cyclodextrin$ and aspirin were studied by FT-IR UN, $^1H$ NMR. $^{13}C NMR$. and FAB-MS spectroscopy in solution and solid state, A stable solid inclusion complex was prepared by the recrystallization method, From the spectral changes of the host and guest molecules, orientational preference for binding in the cyclodextrin cavity was determined.

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Solution and Solid-state Vanadium-51 NMR Studies of Vanadium (V) Complexes

  • Lee, Man-Ho
    • Journal of the Korean Magnetic Resonance Society
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    • v.1 no.1
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    • pp.1-6
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    • 1997
  • Several dioxovanadate (V) complexes are synthesized and studied by solution and solid-state 51V NMR spectroscopy. In the results, large 51V chemical shift anisotropy ({{{{ DELTA delta }}a = -800 ∼720 ppm) and quadrupole coupling (e2q /h = 7.50 ∼ 9.16 MHz) were observed in the solid-state complexes. The isotropic chemical shifts of the solid samples are very close to the values obtained from solution measurements.

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Synthesis and Characterization of Novel pH-Sensitive Hydrogels Containing Ibuprofen Pen dents for Colon-Specific Drug Delivery

  • Mahkam, Mehrdad;Poorgholy, Nahid;Vakhshouri, Laleh
    • Macromolecular Research
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    • v.17 no.9
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    • pp.709-713
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    • 2009
  • The aim of this study was to develop novel intestinal specific drug delivery systems with pH sensitive swelling and drug release properties. The carboxyl group of ibuprofen was converted to a vinyl ester group by reacting ibuprofen and vinyl acetate as an acylating agent in the presence of catalyst. The glucose-6-acrylate-1, 2, 3, 4-tetraacetate (GATA) monomer was prepared under mild conditions. Cubane-1, 4-dicarboxylic acid (CDA) linked to two 2-hydroxyethyl methacrylate (HEMA) group was used as the crosslinking agent (CA). Methacrylic-type polymeric prodrugs were synthesized by the free radical copolymerization of methacrylic acid, vinyl ester derivative of ibuprofen (VIP) and GATA in the presence of cubane cross linking agent. The structure of VIP was characterized and confirmed by FTIR, $^1H$ NMR and $^{13}C$ NMR spectroscopy. The composition of the cross-linked three-dimensional polymers was determined by FTIR spectroscopy. The hydrolysis of drug polymer conjugates was carried out in cel-lophane membrane dialysis bags, and the in vitro release profiles were established separately in enzyme-free simulated gastric and intestinal fluids (SGF, pH 1 and SIF, pH 7.4). The detection of a hydrolysis solution by UV spectroscopy at selected intervals showed that the drug can be released by hydrolysis of the ester bond between the drug and polymer backbone at a low rate. Drug release studies showed that increasing the MAA content in the copolymer enhances the rate of hydrolysis in SIP. These results suggest that these polymeric prodrugs can be useful for the release of ibuprofen in controlled release systems.