• Title/Summary/Keyword: NMR spectra

Search Result 667, Processing Time 0.033 seconds

Spectrophotometric Determination of Ephedrine Alkaloids by Charge-Transfer Complexation (전하이동 착물형성에 의한 Ephedrine Alkaloids의 분석화학적 연구)

  • 옥치완;백채선
    • YAKHAK HOEJI
    • /
    • v.31 no.5
    • /
    • pp.330-337
    • /
    • 1987
  • The weak UV absorbing ephedrine alkaloids such as ephedrine, pseudoephedrine, methylephedrine and norephedrine could be analyzed by charge-transfer spectrophotometric method. The results obtained are summarized as follows: (1) It was possible to determine a weak UV absorbing ephedrine alkaloids using the intense charge-transfer UV bands in chloroform. (2) This method was suitable for the spectrophotometric determination of ephedrine alkaloids in mixed pharmaceutical preparation. (3) Linear relationship was found between absorbance and concentration in the range of 1.0$\times$$10^{-5}M$~5$\times$$10^{-5}M$ of ephedrine ($\varepsilon$= 2.72$\times$$10^{4}LM^{-1}cm^{-1}$ and pseudoephedrine ($\varepsilon$=2.84$\times$$10^{4]LM^{-1}cm^{-1}$), 1.0$\times$$10^{-5}M$~5$\times$$10^{-5}$M of methylephdrine ($\varepsilon$=1.68$\times$$10^{4}LM^{-1}cm^{-1}$) and 1/3$\times$$10^{-4}M$~4/3$\times$$10^{-4}M$ of norephedrine ($\varepsilon$=0.74$\times$$10^{4}LM^{-1}cm^{-1}$. (4) CT- complex of ephedrine, pseudoephedrine and methylephedrine has absorption maxima at 293nm and norephedrine have absorption maximum at 253nm. (5) CT-complexes were formed in a 1:1 ratio between ephedrine alkaloids and iodine in chloroform. (6) By UV, IR, and $^1H$-NMR spectra, it could be inferred that CT-complexes were formed by interaction between the basic nitrogen of ephedrine alkaloids as electron (n) donor and iodine as electron ($\sigma$) acceptor.

  • PDF

Effect of Extract from Paeoniae radix on Rabbit Platelets (작약 추출물의 혈소판 작용에 관한 연구)

  • 박영현;손동주
    • Journal of the Korean Society of Food Science and Nutrition
    • /
    • v.31 no.3
    • /
    • pp.511-515
    • /
    • 2002
  • Paeoniae radix has been considered as one of the most important crude drugs used in traditional oriental medicine and has been employed as a circulatory tonic in care of weakness, night sweats, and lumbar pain, etc. Platelet activation plays an important role in thrombosis and haemostasis. Active compounds for the inhibition of platelet activation from Paeoniae radix were extracted and fractionated into five fractions. Its fraction two and three of ethyl acetate extract inhibited the aggregation of washed rabbit platelets induced by collagen. Two active compounds, bezoyloxypaeoniflorin and paeoniflorin, were isolated from fraction two and three by silica gel column and high performance liquid chromatography. The chemical structures were determined by comparison of their proton and carbon nuclear magnetic resonance spectra. Benzoyloxypaeoniflorin showed strong inhibition at the concentration of 100 ug/mL against collagen-induced washed rabbit platelets aggregation. It is suggested that Paeoniae radix has become food material to prevent a cardiovascular disease.

Preparation and Characterization of Swallow-Tail Terrylene Bisimide as Organic Phosphor (Swallow-Tail Terrylene Bisimide 적색 유기 형광체 제조 및 특성 연구)

  • Jung, Sung Bong;Jeong, Yeon Tae
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
    • /
    • v.33 no.3
    • /
    • pp.194-200
    • /
    • 2020
  • Perylene bisimide derivatives are developed for red organic phosphor because of their advantages, such as excellent luminous efficiency and high thermal stability. Despite these advantages, they have poor solubility characteristics in organic solvents and short emission wavelength as red organic phosphor for hybrid light-emitting diodes (LEDs). In this study, we prepared terrylene bisimide using a coupling reaction and swallow-tail imide group, which has excellent solubility. The structures and properties of swallow-tail terrylene bisimide (9C) were analyzed using 1H-nuclear magnetic resonance (1H-NMR), Fourier-transform infrared (FT-IR), UV/Vis spectroscopy, and thermal gravimetric analysis (TGA). The maximum absorption wavelength of (9C) in the UV/Vis spectrum was 647 nm, and the maximum emission wavelength was 676 nm. In the TGA, (9C) demonstrated good thermal stability with less than 5 wt% weight loss up to 415℃. In the solubility test, (9C) has a good solubility of more than 5 wt% in chloroform and dichloromethane. When the compounds (9C) were mixed with PMMA (polymethly methacrylate), the films showed peaks at 680 nm in the PL spectra. The results verify the suitability of (9C) as a red organic phosphor for hybrid LEDs.

CORRELATION BETWEEN BIS-GMA : TEGDMA RATIO AND DEGREE OF CONVERSION IN VARIOUS LAYERS OF COMPOSITE AFTER ADDITIONAL HEAT CURING (수종 복합레진 내의 bis-GMA와 TEGDMA의 구성비가 레진 인레이 법에 의한 부가적 열처리시 복합레진의 표면 및 내부의 중합률 변화에 미치는 영향)

  • Park, Seong-Ho;Chung, Chan-Moon
    • Restorative Dentistry and Endodontics
    • /
    • v.21 no.2
    • /
    • pp.642-651
    • /
    • 1996
  • The purpose of this study was to evaluate the relationship between monomer compositions and the changes in the degree of conversion in the various layers of composites after additional heat curing. Four types of composites and 3 types of inlay ovens were used in this study. Composite was placed in a 4-mm thick teflon mold, and light cured from the top for 60 seconds. Ten samples were prepared for each composite ; 5 of these were additionally heat cured in an inlay oven as the manufacturer recommended. After light curing or light and heat curing, the samples were sectioned into four parts and assigned to groups A, B, C, or D according to their distance from the light source. These sections were then thinned to 50-$70{\mu}m$, and these wafers were analyzed with a Fourier Transform Infrared Spectrometer(FI-IR) to determine the degree of conversion. A standard baseline technique was used to calculate the degree of conversion. $^{13}C$ NMR spectra of bis-GMA, TEGDMA and bis-EMA, were acquired using a Varian Gemini spectrometer operated at 200 MHz. $CDCl_3$ solvent was used for qualitative analysis. The degree of conversion was affected by bis-GMA : TEGDMA ratio but it seemed to be also affected by other factors. When the composites were heat cured, significant increases in the degree of conversion were noted throughout the samples, but the amount of increase differed between materials. Thus, clinical performance of a heat-treated composite inlay may be different depending on materials.

  • PDF

Kinetics of Malonyl-CoA Synthetase from Rhizobium trifolii and Evidences for Malonyl-AMP Formation as a Reaction Intermediate

  • Kang, Sang-Won;Hong, Sung-Yu;Ryoo, Hyung-Don;Rhyu, Gyung-Ihm;Kim Yu-Sam
    • Bulletin of the Korean Chemical Society
    • /
    • v.15 no.5
    • /
    • pp.394-399
    • /
    • 1994
  • The catalytic mechanism of malonyl-CoA synthetase from Rhizobium trifolii was investigated by the steady state kinetics and intermediate identification. Initial velocity studies and the product inhibition studies with AMP and PPi strongly suggested ordered Bi Uni Uni Bi Ping-Pong Ter Ter system as the most probable steady state kinetic mechanism of malonyl-CoA synthetase. Michaelis constants were $0.17{\pm}0.04 {\mu}M,\;0.24{\pm}0.18 {\mu}M\;and\;0.045{\pm}0.26 {\mu}$M for ATP, malonate and CoA, respectively. The TLC analysis of the $^{32}P-labelled$ products in reaction mixture containing $[{\gamma}-^{32}P]$ ATP in the absence of CoA showed that PPi was produced after the sequential addition of ATP and malonate. Formation of malonyl-AMP, suggested as an intermediate in the kinetically deduced mechanism, was confirmed by the analysis of $^{31}P-NMR$ spectra of AMP product isolated from the $^{18}O$ transfer experiment using $[^{18}O]$malonate. Two resonances were observed, corresponding to AMP labelled with zero and one atom of $^{18}O$, indicating that one atom of $^{18}O$ transferred from $[^{18}O]$malonate to AMP through the formation of malonyl-AMP. Formation of malonyl-AMP was also confirmed through the TLC analysis of reaction mixture containing $[{\alpha}-^{32}P]$ATP. These results strongly support the ordered Bi Uni Uni Bi Ping-Pong Ter Ter mechanism deduced from the initial velocity and product inhibition studies.

Synthesis and Antitumor Evaluation of N-Alkyl-N-Nitrosocarbamoyl-$\alpha$-Amino- and 3$\beta$-Amino-$\alpha$-Cholestane Derivatives (N-Alkyl-N-Nitrosocarbamoyl-3$\alpha$-Amino-와 3$\beta$-Amino-5$\alpha$-Cholestane 유도체들의 합성 및 항암작용 평가)

  • 김정균;최순규;조인섭;유동식;유성호;문경호
    • YAKHAK HOEJI
    • /
    • v.29 no.2
    • /
    • pp.62-69
    • /
    • 1985
  • The isomeric intermediates, $3{\alpha}$and $3{\beta}-amino-5{\alpha}-cholestane required for the synthesis of N-nitrosoureas, N-(2-chloroethyl)-N-nitrosocarbamoyl-$3{\alpha}-amino-5{\alpha}$-cholestane (9), N-methyl-N-nitrosocarbamoyl-3${\alpha}-amino-5{\alpha}-cholestane$ (10), N-(2-chloroethyl)-N-nitrosocarbamoyl-$3{\beta}-amino-5{\alpha}-cholestane$: (7), and N-methyl-N-nitrosocarbamoyl-$3{\beta}-amino-5{\alpha}-cholestane$ (8) were obtained through the $LiAlH_{4}$ reduction of $5{\alpha}$-cholestan-3-one oxime, followed by the chromatographic separation: the assignment of the stereochemistry of both isomers were based on the shape and chemical shift of $C_{3}$-proton resonances on their NMR spectra and on the elution mobility on the TLC. The urea intermediates, N-(2-chloroethyl) carbamoyl-3.alpha.-amino-5.alpha.-cholestane (13), N-methylcarbamoyl-$3{\alpha}-amino-5{\alpha}-cholestane$ (14), N-(2-chloroethyl) carbamoyl-$3{\beta}-amino-5{\alpha}-cholestane (11) and N-methyl-$3{\beta}-amino-5{\alpha}$-cholestane (12) were prepared by the treatment of each isomers ($3{\alpha}$-amino-and $3{\beta}-amino-5{\alpha}$-cholestane) with alkyl isocyanates in anhydrous $CHCl_{3}$, and the corresponding nitrosoureas, 7-10 were obtained by the nitrosation of the ureas, 11-14, with AcOH (or HCOOH)/$NaNO_{2}$ in ice-cold condition. The inhibitory activity of the nitrosoureas, 7-10, and their intermediates, 12-14 towards the growth of L1210 murine leukemia cells, were examined. Among them, the compounds 9 and 10 exhibited high activity having $ED_{50}$ to be 5.5g/ml and 6.1g/ml, respectively.

  • PDF

Synthesis and Characterization of Swallow-Tail Perylene Bisimide as Organic Phosphor for Hybrid LED (Hybrid LED용 유기 형광체로서의 Swallow-Tail Perylene Bisimide 제조 및 특성 연구)

  • Jung, Sung Bong;Jeong, Yeon Tae
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
    • /
    • v.32 no.1
    • /
    • pp.86-92
    • /
    • 2019
  • Although perylene bisimide derivatives have advantages such as excellent thermal stability and high luminance efficiency, they have poor solubility characteristics in organic solvents. In this research, in order to improve the solubility characteristics, we prepared perylene bisimide derivatives (1C) and (2C) with swallow-tail substituted imide, which is known to lead to excellent solubility. The structures and properties of swallow-tail perylene bisimide (1C) and (2C) were analyzed by $^1H-NMR$, FT-IR, UV/Vis spectroscopy, and thermogravimetric analysis (TGA). The maximum absorption wavelengths of (1C) and (2C) in the UV/Vis spectrum were 558 nm and 556 nm, respectively, and the maximum emission wavelengths were 602 nm and 600 nm, respectively. In the TGA, (1C) demonstrated good thermal stability with less than 5 wt% weight loss up to $242^{\circ}C$. In the solubility test, (1C) and (2C) exhibited solubilities of more than 5 wt% in chloroform, ethyl acetate, and dimethylformamide, but not in methanol. When the compounds (1C) and (2C) were mixed with PMMA (polymethyl methacrylate), thin films showed peaks at 679 nm and 677 nm, respectively, in the photoluminescence spectra. (1C) was found to be a possible candidate as red organic phosphor for hybrid LEDs.

A detailed study of physicochemical properties and microstructure of EmimCl-EG deep eutectic solvents: Their influence on SO2 absorption behavior

  • Zhu, Jiahong;Xu, Yingjie;Feng, Xiao;Zhu, Xiao
    • Journal of Industrial and Engineering Chemistry
    • /
    • v.67
    • /
    • pp.148-155
    • /
    • 2018
  • To get a better understanding of the effect of physicochemical properties and microstructure on $SO_2$ absorption behavior of DESs with different molar ratios of EmimCl and EG (from 2:1 to 1:2), densities (${\rho}$), viscosities (${\eta}$), speeds of sound (u), refractive indices ($n_D$), and thermal decomposition temperatures ($T_d$) of EmimCl-EG DESs were measured and used to obtain the other derived properties, such as thermal expansion coefficient (${\alpha}_p$) and activation energy for viscous flow ($E_{\eta}$). Moreover, FT-IR spectra and in situ variable-temperature NMR spectroscopy were employed to study the microstructures of DESs. Based on physicochemical and spectroscopic properties, the influence of the concentrations of EmimCl on the interactions in DESs was explored to be associated with their $SO_2$ absorption behavior. The results show that the interactions between $Emim^+$ and $Cl^-$ of EmimCl is gradually weakening with increasing the concentration of EG in DESs by forming of hydrogen bond interaction of $O-H{\cdots}Cl^-$, resulting in a decrease of ${\rho}$, ${\eta}$, u, $n_D$, and $T_d$ of DESs, and hindering the charge-transfer interaction of $SO_2$ with $Cl^-$ and deceasing $SO_2$ capture capacity. Moreover, the $SO_2$ absorption capacity of DESs is proportional to their ${\rho}$ and $E_{\eta}$, respectively.

The Effect of Gingko Biloba Extract on Energy Metabolic Status in C3H Mouse Fibrosarcoma : Evaluated by in vivo $^{31}P$ Magnetic Resonance Spectroscopy (Gingko biloba extract가 C3H 마우스 섬유육종의 에너지 대사 상태에 미치는 영향 : 생체내 $^{31}P$ 자기공명 분광법을 이용한 분석)

  • Ha Sung Whan;Kim Won Dong;Ahn Yong Chan;Park Chan Il;Lim Tae Hwan;Lee Tae Kuen
    • Radiation Oncology Journal
    • /
    • v.20 no.2
    • /
    • pp.147-154
    • /
    • 2002
  • Purpose : Gingko biloba extract (GBE), a natural product extracted from Gingko leaves, is known to increase the radiosensitivity of tumors. This radiosensitization probably arises from the increase in the peripheral blood flow by decreasing the blood viscosity and relaxing the vasospasm. The influence of a GBE on the metabolic status in fibrosarcoma II (FSall) of a C3H mouse was investigated using $^{31}P$ magnetic resonance spectroscopy (MRS). Materials and Methods : Eighteen C3H mice with fibrosarcoma II $(from\;100\;mm^3\;to\;130\;mm^3)$ were prepared for this experiment. The mice were divided into 2 groups; one (9 mice) without a priming dose, and the other (9 mice) with a priming dose of GBE. The GBE priming dose (100 mg/kg) was administered by an intraperitoneal (i.p.) injection 24 hours prior to the measurement. First $^{31}P$ MRS spectra were measured in the mice from each group as a baseline and test dose of GBE (100 mg/kg) was then administered to each group. One hour later, the $^{31}P$ MRS spectra were measured again to evaluate the change in the energy metabolic status. Results : In the group without the priming dose, the mean pH, PCr/Pi, PME/ATP, Pi/ATP, PCr/(Pi+PME) values 1 hour after the test dose were not changed significantly compared to the values at the baseline. However, in the group with the priming dose, the mean PCr/Pi, Pi/ATP, PCr/(Pi+PME) values 1 hour after the test dose changed from the baseline values of 0.49, 0.77, 0.17 to 0.74, 0.57, 0.28 respectively. According to the paired t-test, the differences were statistically significant. Conclusion : The above findings suggest that the metabolic status is significantly improved after administering GBE if the priming dose is given 24 hours earlier. This shows that the radiosensitizing effect of GBE is based on the increase of tumor blood flow and the improvement in the metabolic status.

Studies on the Electrochemical Behavior of Heavy Lanthanide Ions and the Synthesis, Characterization of Heavy Metal Chelate Complexes(II). Synthesis and Characterization of Eight Coordinate Tungsten(IV) and Cerium(IV) Chelate Complex (무거운 란탄이온의 전기화학적 거동 및 중금속이온의 킬레이트형 착물의 합성 및 특성에 관한 연구(제2보). 8배위 텅스텐(IV)과 세륨(IV)의 킬레이트형 착물의 합성 및 특성)

  • Kang, Sam Woo;Chang, Choo Wan;Suh, Moo Yul;Lee, Doo Youn;Choi, Won Jong
    • Analytical Science and Technology
    • /
    • v.5 no.1
    • /
    • pp.41-49
    • /
    • 1992
  • An attempt was made to prepare two series of tetrakis eight-coordinate tungsten(IV) and cerium(IV) complexes containing the 5,7-dichloro-8-quinolinol(N:${\pi}$-acceptor atom, O:${\pi}$-donor atom) ligand. Tetrakis eight-coordinate tungsten(IV) complex of 2-mercaptopyrimidine(N:${\pi}$-acceptor atom, S:${\pi}$-donor atom) ligand have also been prepared. And the new series of mixed-ligand eight-coordinate tungsten(IV) complexes containing bidentate ligands 5,7-dichloro-8-quinolinol and 2-mercaptopyrimidine have been prepared, isolated by TLC and characterized. $W(dcq)_4$, $W(dcq)_3(mpd)_1$, $W(dcq)_2(mpd)_2$, $W(dcq)_1W(dcq)_3$ and $W(mpd)_4$ complexes of MLCT absorption band appeared to 710nm, 680nm, 625nm, 581nm, and 571nm(${\varepsilon}\;max={\sim}>{\times}10^4$) on low-energy respectively. The specific absorption wave length of $Ce(dcq)_4$ is appeared 520nm(${\varepsilon}\;max={\sim}>{\times}10^4$). The Chemical shift values by proton of coordinated position appeared to $W(dcq)_4$ [$H_2:8.9ppm$]; $W(dcq)_3(mpd)_1$ [$H_2:9.3$,$H_6:9.2ppm$]; $W(dcq)_2(mpd)_2$ [$H_2:9.7$,$H_6:8.95ppm$]; $W(dcq)_1(mpd)_3$ [$H_2:9.8$,$H_6:9.4ppm$]; $W(mpd)_4$ [$H_6:8.8ppm$]; $Ce(dcq)_4$ [$H_2:9.3ppm$] with $^1H$-NMR. The inertness of mixed-ligand eight coordinate tungsten(IV) complexes have been investigated by UV-Vis. spectroscopic method in dimethylsulfoxide at $90^{\circ}C$. The inertness of $W(dcq)_n(mpd)_{4-n}$ complexes showed the following order, $W(dcq)_3(mpd)_1;k_{obs.}=3.8{\times}10^{-6}$ > $W(mpd)_4;k_{obs.}=6.0{\times}10^{-6}$ > $W(dcq)_4;k_{obs.}=6.4{\times}10^{-6}$ > $W(dcq)_2(mpd)_2;k_{obs.}=7.0{\times}10^{-6}$ > $W(dcq)_1(mpd)_3;k_{obs.}=1.7{\times}10^{-5}$, which showed the inertness until 16days, 10days, 9days, 8days, and 4days. The $W(mpd)_4$ is very inert as $k_{obs.}=3.6{\times}10^{-6}$(16days) in xylene at $90^{\circ}C$ and $k_{obs.}=6.0{\times}10^{-6}$(10days) in DMSO at $90^{\circ}C$.

  • PDF