• 제목/요약/키워드: $^1H$ nuclear magnetic resonance

검색결과 308건 처리시간 0.029초

Solution Nuclear Magnetic Resonance Spectral Characterization of Iron(II) Porphyrin Complexes of Weakly Coordinating Anions

  • Song, Byung-Ho;Park, Bong-Jin;Han, Chul-Hee
    • Bulletin of the Korean Chemical Society
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    • 제23권1호
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    • pp.119-122
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    • 2002
  • Weakly coordinating anions show little affinity for binding to unfunctionalized iron(II) porphyrins. The electron-deficient 5, 10, 15, 20-tetrakis(pentafluorophenyl)porphinatoiron(II) compound is utilized in this study to demonstrate solution coordination by chloride, bromide and acetate ions. The binding strength of anions to the iron(II) porphyrin is reflected by a systematic change in pyrrole proton chemical shift in $^1H$ NMR spectra; the pyrrole resonance moves downfield when the ${\sigma}$-donor ability of anions is decreased.

Flavanone 3β-Hydroxylases from Rice: Key Enzymes for Favonol and Anthocyanin Biosynthesis

  • Kim, Jeong Ho;Lee, Yoon Jung;Kim, Bong Gyu;Lim, Yoongho;Ahn, Joong-Hoon
    • Molecules and Cells
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    • 제25권2호
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    • pp.312-316
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    • 2008
  • Flavanone $3{\beta}$-hydroxylases (F3H) are key enzymes in the synthesis of flavonol and anthocyanin. In this study, three F3H cDNAs from Oryza sativa (OsF3H-1 ~3) were cloned by RT-PCR and expressed in E. coli as gluthatione S-transferase (GST) fusion proteins. The purified recombinant OsF3Hs used flavanone, naringenin and eriodictyol as substrates. The reaction products with naringen and eriodictyol were determined by nuclear magnetic resonance spectroscopy to be dihydrokaempferol and taxifolin, respectively. OsF3H-1 had the highest enzymatic activity whereas the overall expression of OsF3H-2 was highest in all tissues except seeds. Flavanone $3{\beta}$-hydroxylase could be a useful target for flavonoid metabolic engineering in rice.

The Effect of Salt and pH on the Phase Transition Behaviors of pH and Temperature-Responsive Poly(N,N-diethylacrylamide-co-methylacrylic acid)

  • Liu, Tonghuan;Fang, Jian;Zhang, Yaping;Zeng, Zhengzhi
    • Macromolecular Research
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    • 제16권8호
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    • pp.670-675
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    • 2008
  • A series of pH and temperature-responsive (N,N-diethylacrylamide-co-methylacrylic acid) copolymers were synthesized by radical copolymerization and characterized by elemental analysis, Fourier-transform infrared (FT-IR), nuclear magnetic resonance (NMR) $^1H$, $^{13}C$ and LLS. The effects of salt and pH on the phase transition behaviors of the copolymers were investigated by uv. With increasing NaCl concentration, significant salt effects on their phase transition behaviors were observed. UV spectroscopic studies showed that the phase transition became faster with increasing NaCl concentration. In addition, the phase transition behaviors of copolymers were sensitive to pH. The pH and temperature sensitivity of these copolymers would make an interesting drug delivery system.

매실추출물로부터 항균물질의 분리 및 구조동정 (Separation and Identification of Antimicrobial Substances from Prunus mume extract)

  • 박우포;이승철;김성용;최성길;허호진;조성환
    • 한국식품저장유통학회지
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    • 제15권6호
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    • pp.878-883
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    • 2008
  • 항균력이 탁월한 매실추출물로부터 항균활성물질을 column chromatography를 이용하여 순수하게 분리하고, nuclear magnetic resonance (NMR) spectrophtometer 측정기에 의하여 항균활성물질의 화학구조를 다음과 같이 분리 동정하였다. 즉, 매실추출물을 상온에서 메탄올에 현탁한 후, ethyl ether, ethyl acetate, n-butanol로 각각 분배 추출하여 각 용매의 수용성 추출물을 획득하였다. 각 용매의 수용성 추출물을 loading한 후, silica gel(70-230 mesh, Merck) column chromatography하여 소획분을 얻었다. 분리된 분획 중 항균력이 있는 소획분을 Sephadex LH 20을 충진하고 column chromatography하여 각 항균분획물질을 분리하였다. column chromatography에서 분리한 각 항균분획물질(Compound A, Compound B, Compound C)의 구조분석을 위해 $^{1}H$$^{13}C$ NMR 스펙트럼을 실온에서 측정하였다. NMR은 Bruker DRX500 (500MHz)을 이용하여 측정하였으며, 용매와 기준물질은 $CDCl_3$와 TMS를 각각 사용하였다. 이와같이 분리한 각 항균분획물질을 NMR 분석법으로 동정한 결과, isoeugenol, nomilin 및 $\beta$-sitosterol 등으로 확인되었다.

상대습도에 따른 비정질 규산염 나노입자의 함수량 정량 분석을 위한 1H 고상 핵자기 공명 분광분석 방법론 연구 (1H Solid-state NMR Methodology Study for the Quantification of Water Content of Amorphous Silica Nanoparticles Depending on Relative Humidity)

  • 오솔비;김현나
    • 광물과 암석
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    • 제34권1호
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    • pp.31-40
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    • 2021
  • 명목상의 무수 광물의 수소 원자는 격자의 결함에 존재하는 것으로 알려져 있지만, 나노 스케일 입자의 경우 입자 표면에 물과 수산기의 형태로 존재할 수 있다. 본 연구에서는 비정질 규산염 나노입자의 수소 원자 환경에 대한 정량 측정 방법으로서, 1H 고상 핵자기 공명(solid-state nuclear magnetic resonance, NMR) 분광분석의 실효성을 알아보고자 하였다. 온도와 습도가 조절되는 글러브 박스 내에서 NMR 로터에 패킹된 비정질 규산염 나노입자를 25%와 70 % 상대습도에서 2일에서 10일까지 동안 보관한 후 1H NMR 스펙트럼을 측정한 결과, 약간의 차이는 있었으나 큰 변화가 관찰되지 않았다. 이는 NMR 로터에 패킹된 시료의 수소 원자 환경이 외부 대기에 의해 거의 변화하지 않았음을 의미한다. 수화 시간에 따른 비정질 규산염 나노입자의 함수량은 약 10 % 범위에서 차이를 보이며, 이는 글러브 박스의 시간적, 공간적 습도 불균일성에 의한 것으로 생각된다. 1H NMR 스펙트럼의 정량 분석 결과, 수화 상대습도가 증가함에 따라 비정질 규산염 나노입자의 수소 원자 수 역시 선형적으로 증가하였다. 이와 같은 결과는 NMR 로터의 시료 밀폐 능력이 수화 환경을 보존하며, 대기 상대습도 변화에 따른 나노입자의 함수량 변화 측정에 적합함을 의미한다. 본 연구의 결과를 통해, 1H 고상 핵자기 공명 분광분석을 이용하여 나노 스케일의 명목상의 무수 광물의 표면적, 결정도가 습도에 따른 광물의 함수량 변화에 미치는 영향에 대한 체계적인 연구를 할 수 있을 것으로 기대된다.

식용식물의 항산화 효과 검색과 산초의 항산화 성분 (Further Screening for Antioxidant Activity of Vegetable Plants and Its Active Principles from Zanthoxylum schinifolum)

  • Mun, Sook-Im;Ryu, Hong-Soo;Lee, Hee-Jung;Park, Jae-Sue
    • 한국식품영양과학회지
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    • 제23권3호
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    • pp.466-471
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    • 1994
  • The antioxidant activity of methanol extracts of thirty plants was tested using the methol of 1, 1-diphenyl-2-pi-cryl hydrazyl (DPPH) reactivity. Four methanol extracts from Zingiber officinale, Piper nigrum , Zanthoxylum schinifolium and Capsocum annuum were found to be the most effective on DPPH radical scavenging activity. The next effective ones were Perilla frutescens , Sedium sarmentosum , Raphnus sativas, aArctium lappa, Beta vulgaris. Brassica oleracea var. Acephala, bBrassica juncea inorder, and the others did not show a considerable activity. The methanol extract obtained from the seed coats of Zanthoxylum schinifolium was fractinated with several sovlents. The interphase materials exhibited the strongest antioxidant activity and was further purified by silica gel and Sephadex LH-20 column chormatography. Two active principles were isolated and identified as quercetin -3-O-$\alpha$-L-rhamonopyranoiside(quercitrin) and quercetin 3-O-$\alpha$-D-galactopyranoside (hyperoside) by ultraviolet(UV), proton nuclear magetic resonance (1H-NMR) and carbon nuclear magnetic resonance (13C-NMR). Its antioxidative activity was a little higher that that of L-ascorbic acid.

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Low-ε Static Probe Development for 15N-1H Solid-state NMR Study of Membrane Proteins for an 800 MHz NB Magnet

  • Park, Tae-Joon;Choi, Sung-Sub;Jung, Ji-Ho;Park, Yu-Geun;Kim, Yongae
    • Bulletin of the Korean Chemical Society
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    • 제34권3호
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    • pp.823-826
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    • 2013
  • A low-${\varepsilon}$ solid-state NMR(Nuclear Magnetic Resonance) probe was developed for the spectroscopic analysis of two-dimensional $^{15}N-^1H$ heteronuclear dipolar coupling in dilute membrane proteins oriented in hydrated and dielectrically lossy lipid environments. The system employed a 800 MHz narrow-bore magnet. A solenoid coil strip shield was used to reduce deleterious RF sample heating by minimizing the conservative electric fields generated by the double-tuned resonator at high magnetic fields. The probe's design, construction, and performance in solid-state NMR experiments at high magnetic fields are described here. Such high-resolution solid-state NMR spectroscopic analysis of static oriented samples in hydrated phospholipid bilayers or bicelles could aid the structural analysis of dilute biological membrane proteins.

초음파 개질 경유의 연료특성과 연소특성의 상관관계에 관한 연구 (II) -화학구조와 세탄가의 상관성- (A Study on Relationship between Fuel Characteristics and Combustion Characteristics of Reformed Diesel Fuels by Ultrasonic Energy Irradiation (II) - Relationship between Chemical Structure and Cetane Number -)

  • 이병오;류정인
    • 한국자동차공학회논문집
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    • 제11권1호
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    • pp.64-71
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    • 2003
  • In order to analyze the effect of the chemical structure and the cetane number of reformed diesel fuels by ultrasonic energy irradiation, proton nuclear magnetic resonance spectrometer$(^1H-NMR)$ was used. From the study, following conclusive remarks can be made. 1) Branch Index(BI), aromatics percentages, and alpha methyl radical$(H_{\alpha})$ of the reformed diesel fuels by ultrasonic energy irradiation decreased more than the conventional ones. 2) All the cetane numbers which were calculated from carbon type structure and hydrogen type distribution of the reformed diesel fuels increased more than the conventional ones. 3) It is more reasonable to predict cetane number equation from carbon type structure than from hydrogen type distribution. 4) BI, aromatics percentages, and $H_{\alpha}$ on both for conventional fuel and reformed diesel fuels by ultrasonic energy irradiation are inversely proportional to cetane number fur these fuels.

A Solid-State NMR Study of Water in Poly(vinyl butyral) by Magic Angle Spinning

  • Jeong, Soon-Yong;Han, Oc-Hee
    • Bulletin of the Korean Chemical Society
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    • 제28권4호
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    • pp.662-666
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    • 2007
  • Poly(vinyl butyral) (PVB) with different wt% water was studied gravimetrically as well as with 1H magic angle spinning (MAS) nuclear magnetic resonance (NMR). The composition of PVB samples changes during MAS NMR because of the centrifugal force. As MAS time progresses, initially free water was removed fast but bound water also was gradually depleted. More water was diminished at faster spinning speeds, longer spinning time, higher temperatures, and higher initial water contents. As water in PVB was reduced, the chemical shifts and line widths of different types of water and also those of PVB changed. Our results demonstrate that 1H MAS NMR carried out at 10 kHz in less than about 5 minutes is a convenient and sensitive technique to measure: (a) the content variations of different types of water in polymers, (b) the degree of the interaction of water and polymer, and (c) the molecular dynamics of the polymer. Our study can be extended to different soft polymers with other small molecules than water in them.

펄스방식의 핵자기 공명장치에 관한 새로운 구현방법 (New Implementation Method of the Pulsed Nuclear Magnetic Resonance Apparatus)

  • 김청월
    • 전자공학회논문지C
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    • 제35C권10호
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    • pp.1-11
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    • 1998
  • 본 논문은 핵자기 공명신호를 검출하기 위하여 자석상자 내에 한 개의 코일을 가진 펄스방식의 핵자기 공명장치에 대한 새로운 구현방법에 관한 것이다. 수소 원자핵의 Larmor 주파수가 5MHz가 되도록 설계된 자석상자에 5MHz 고주파 자기장을 인가하여 자석상자 내에 투입된 글리세린 시료로부터 수소 원자핵의 공명신호를 얻었다. 자석상자 내의 정자기장은 자기장의 세기가 1168 gauss인 영구자석을 사용하여 만들었으며, 고주파 자기장은 5MHz의 주파수를 가지며 전류의 크기가 8A인 고주파 신호를 5.73μH의 코일에 인가하여 발생시켰다. 고주파 자기장의 발생시간을 2.8μsec로 하였을 때 핵자기 공명신호는 최대 크기로 나타났으며, 반복 검출을 하기 위하여 고주파 자기장의 발생주기를 100msec로 설계하였다. 시료에서 발산되어 자석상자 내의 코일에 감지되는 핵자기 공명신호는 Larmor 주파수와 같은 주파수를 가지는 신호가 진폭변조된 형태로 나타났다. 코일에 감지된 신호를 송수신 분리회로와 전치증폭기 및 중간증폭기에서 각각 20.7dB, 36dB 및 40dB로 증폭하고 동기검파회로에서 검파하여 핵자기 공명신호를 얻었다.

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