• 제목/요약/키워드: Complex mixtures

검색결과 179건 처리시간 0.024초

한개의 산소다리를 가진 몰리브덴(V) 착물의 산소고리화 반응 (II). 2성분 혼합용매에서 용매물과 $[Mo_2O_3(Phen)_2(NCS)_4]$의 반응 (Oxygen Ring Formation Reaction of Mono-Oxo-Bridged Binuclear Molybdenum(V) Complex (II). Reaction of $[Mo_2O_3(Phen)_2(NCS)_4]$ with Solvent Water in Water + Co-Solvent Mixtures)

  • 오상오;석휘영
    • 대한화학회지
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    • 제32권3호
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    • pp.203-210
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    • 1988
  • 물-아세톤, 물-아세토니트릴 및 물-디메틸포름아미드의 2성분 혼합용매중에서 한개의 산소다리로 된 이핵몰리브텐(V)착물, $[Mo_2O_3(Phen)_2(NCS)_4]$은 두개의 산소다리로 된 이핵 몰리브텐(V)착물, $[Mo_2O_4(Phen)_2(NCS)_2]$을 생성한다. $[Mo_2O_3(Phen)_2(NCS)_4]$$[Mo_2O_4(Phen)_2(NCS)_2]$로 바뀌는 속도는 분광광도법으로 측정하였다. 이 때 온도는 $10^{\circ}C$에서 $40^{\circ}C$, 압력은 1bar에서 1500bar로 변화시켰다. 속도상수는 물의 농도 증가에 따라 증가하였다. 수소이온농도의 증가에 따라서는 감소하였다. 여러가지 공용매에서 산소고리화 반응속도는 유전상수$({\varepsilon}/{\varepsilon}_0)$의 증가와 같이 ACT < AN < DMF의 순으로 증가하였다. 관찰된 음의 활성화엔트로피($[\Delta}S^{\neq}$), 활성화부피($[\Delta}V^{\neq}$) 및 활성화 압축율(${\Delta}{\beta}^{\neq}$) 값은 착물이 전이상태에서 용매 물분자를 강하게 당기는 회합성메카니즘임을 알게 한다.

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$Zn[BH_4]_2$ 분말의 합성과 열분해 특성 (Synthesis and thermal decomposition of $Zn[BH_4]_2$)

  • 전은;조영환
    • 한국수소및신에너지학회논문집
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    • 제16권3호
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    • pp.262-268
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    • 2005
  • [ $Zn(BH_4)_2$ ](8.4 wt% theoretical hydrogen storage capacity powders have been successfully synthesized by mechanochemical reaction from mixtures of $ZnCl_2$ and $NaBH_4$ powders in a 1:2 molar ratio in different times. $$ZnCl_2+2NaBH_4{\rightarrow}Zn(BH_4)_2+2NaCl$$ (1) $Zn(BH_4)_2$ powders were characterized by X-ray diffractometry(XRD), and Furier Transform Infrared spectrometry(FT-IR). The thermal stabilities of $Zn(BH_4)_2$ powders were studied by Differential scanning calorimetry(DSC), Thermogravimetry analysis(TGA), and Mass spectrometry(MS). $Zn(BH_4)_2$ can be tested for hydrogen evolution without further purification. The reaction to yield hydrogen is irreversible, the other products being compounds of Zn, and borane. $Zn(BH_4)_2$ thermally decomposes to release borane and hydrogen gas between about 85 and 150$^{\circ}C$.

MALDI Mass Spectrometric Analysis of Nonderivatized Steroids Using Cyclodextrin-supported 2,5-Dihydroxybenzoic Acid as Matrix

  • Son, Jeongjin;Cha, Sangwon
    • Bulletin of the Korean Chemical Society
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    • 제35권5호
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    • pp.1409-1412
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    • 2014
  • Sex hormones are important metabolites in vertebrates' development and reproduction. For rapid screening sex hormones, matrix-assisted laser desorption/ionization (MALDI) mass spectrometry (MS) is one of the promising analytical platforms, but MALDI MS faces many challenges in detecting steroids such as low ionization efficiency and matrix background interference. One potential strategy to overcome matrix interference in the low m/z region is using a cyclodextrin (CD)-supported matrix for steroid analysis since CD-supported matrixes are known to effectively suppress matrix-related ion signals. In this study, we aimed to find the optimal CD-supported matrix for the analysis of the nonderivatized sex steroids. Our results showed that the ${\alpha}CD$-supported 2,5-dihydroxybenzoic acid (DHB) matrix efficiently ionized all three major classes of sex hormones, estrogens, androgens, and progestagens, with low or no matrix background and also with high sensitivity. In addition, the ${\alpha}CD$-supported DHB matrix mainly generated molecular ions or protonated ions of sex hormones, and this enabled us to obtain information-rich tandem mass spectra which potentially lead to unambiguous identification of steroid species from complex metabolite mixtures.

관형 연소기의 열-음향 진동에 의한 소음 특성 예측 (Prediction of Thermo-acoustic Oscillation Characteristics in a Ducted Combustor)

  • 김재헌;이정한;이수갑;정인석
    • 한국음향학회지
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    • 제18권7호
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    • pp.56-66
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    • 1999
  • 일반 내연기관이나 산업용로, 로켓 엔진 등의 기본적인 형상이라고 할 수 있는 관형 연소기에서 발생하는 연소 소음은 열-음향 되먹임 현상에 의해 야기되는 형태가 지배적이며. 심할 경우 시스템의 파괴를 야기할 수도 있는 중요한 문제이다. 본 연구에서는 열-음향 진동중에서도 열-기인 음향 진동으로 분류될 수 있는 현상에 초점을 맞추어 유동장, 음향장 및 연소 반응을 수치적으로 해석하여 여러 주어진 조건에 따른 정상적인 해석뿐만 아니라 음압 수준이나 기본 주파수 예측과 같은 정량적인 결과 도출을 효과적으로 수행할 수 있는 수치적 기법의 개발을 목적으로 하였다. 다양한 당량비를 가진 혼합기에 대해 수치 해석을 수행한 결과 실험 측정치의 경향과 잘 일치할 뿐만 아니라 정량적인 면에서도 상당히 정확한 예측을 할 수 있음을 확인하였다.

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Identification of Xanthium Sibiricum Components using LC-SPE-NMR-MS Hyphenated System

  • Sohn, Ji Soo;Jung, Youngae;Han, Ji Soo;Hwang, Geum-Sook
    • 한국자기공명학회논문지
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    • 제22권2호
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    • pp.26-33
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    • 2018
  • Xanthium sibiricum is used as a traditional folk medicine for the treatment of cancer, fever, headache, nasal sinusitis, and skin pruritus. This study aimed to identify components from Xanthium sibiricum extracts using an SPE-800MHz NMR-MS hyphenated system. The simultaneous acquisition of MS and NMR spectra from the same chromatographic peaks significantly increases the depth of information acquired for the compound and allows the elucidation of structures that would not be possible using MS or NMR data alone. LC -NMR analysis was conducted using a HPLC separation system coupled to 800 MHz spectrometer equipped with a cryoprobe, and a SPE unit was used to automatically trap chromatographic peaks using a HPLC pump. LC-MS analysis was conducted with a Q-TOF MS instrument using ESI ionization in the negative ion mode. Using the hyphenated analysis, several secondary metabolites were identified, such as 3',5'-O-dicaffeoylquinic acid, 1',5'-O-dicaffeoyl- quinic acid, and ethyl caffeate. These results demonstrate that the SPE-800MHz NMR-MS hyphenated system can be used to identify metabolites within natural products that have complex mixtures.

Simultaneous HPLC Analysis of Arachidonic Acid Metabolites in Biological Samples with Simple Solid Phase Extraction

  • Kim, Hyung-Gun;Huh, Young-Na;Park, Kun-Suk
    • The Korean Journal of Physiology and Pharmacology
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    • 제2권6호
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    • pp.779-786
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    • 1998
  • A reversed-phase high-performance liquid chromatogrphy (RP-HPLC) has been developed to analyze the metabolites of arachidonic acid based on the specificities of ultraviolet absorption of these various metabolites and is sensitive to the nanogram level. This procedure makes it possible to extract complex mixtures of eicosanoids efficiently with a single step and to analyze them simultaneously by RP-HPLC from biological samples using octadesylsilyl silica extraction column and $PGB_2$ as an internal standard. The cyclooxygenase products {prostaglandin $(PG)D_2,\;PGE_1,\;PGE_2,\;PGF_{1{\alpha}},\;PGF{2{\alpha}},\;6-keto-PGF_{1{\alpha}},$ and thromboxane $B_2(TXB_2)}$ and lipid peroxidation product, isoprostanes, of arachidonic acid were monitored by one isocratic HPLC system at 195 nm wavelength. The lipoxygenase products ${leukotriene(LT)B_4,\;LTC_4,\;LTD_4,$ and 5-hydroxyeicosatetraenoic acid (5-HETE), 12-HETE, 15-HETE} were measured by another isocratic HPLC system at 280 nm for LTs and 235 nm for HETEs. This method provides a simple and reliable way to extract and assess quantitatively the final arachidonic acid metabolites.

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The Microcosm study for evaluating biobarrier application on sequential degradation of TCE products by Gasoline-Degradaing Mixed Culture

  • Lee, Jae-Sun;Lee, Si-Jin;Lee, Young-Kee;Chang, Soon-Woong
    • 한국생물공학회:학술대회논문집
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    • 한국생물공학회 2003년도 생물공학의 동향(XIII)
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    • pp.440-444
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    • 2003
  • 본 연구에서는 난분해성 물질인 액상의 TCE가 영가철 표면에서 반응시 완전히 분해가 되지 않은 상태에서 생성되어지는 부산물인 Cis-DCE와 VC의 톨루엔 분해균주에 의한 처리 가능성을 회분식 실험으로 관찰하였다. 각각 2ppm의 Cis-DCE와 VC에 톨루엔 균주를 주입한 결과 1차기질로 톨루엔을 사용하고 그후에 Cis-DCE와 VC를 제거 하는 것으로 나타났다. 또한 동시에 주입시 1차기질로 톨루엔을 사용하는 것은 동일하나 VC를 먼저 사용하고 그후에 Cis-DCE를 제거하며 제거 속도 또한 줄여드는 것으로 나타났다.

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생약제제의 등록규정 차별화에 관한 연구 (A Study on the Distinction of Registration Regulations for Herbal Medicines)

  • 주윤정;오정미;한병현;홍성선
    • 한국임상약학회지
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    • 제11권2호
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    • pp.68-77
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    • 2001
  • Herbal medicines have been used since ancient times as medicines to treat and relieve the symptoms of many different human diseases. However, so far, relatively few herbal medicines have been evaluated scientifically to prove their safety, potential benefits and effectiveness. This study was conducted to provide the groundwork for improving the current registration regulations for herbal medicines in distinction from synthetic medicines. The study was performed based on the literature research and individual interviews with 5 experts who had extensive experience in registration of herbal medicines. When compared with synthetic drugs, herbal medicines exhibit some marked differences, namely the active principles are frequently unknown, standardization, stability and quality control are not easy, they are usually mixtures of complex compounds. Second, the current regulations for herbal medicines are reviewed by comparison of foreign regulation systems like the one in China. The regulation requirements of herbal medicine in China are in distinction from synthetic drugs. The authors conclude that new registration requirements for the herbal medicines should be changed as follows; the toxicity and efficacy data should be submitted as mixed herbal preparation and the documents and other research on the reproduction and generation toxicity need to be shown for the proof of reproduction and generation toxicity, if needed.

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Targeted chiral lipidomics analysis of bioactive eicosanoid lipids in cellular systems

  • Lee, Seon-Hwa;Blair, Ian A.
    • BMB Reports
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    • 제42권7호
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    • pp.401-410
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    • 2009
  • We have developed a targeted lipidomics approach that makes it possible to directly analyze chiral eicosanoid lipids generated in cellular systems. The eicosanoids, including prostaglandins (PGs), thromboxanes (TXs), leukotrienes (LTs) and alcohols (HETEs), have been implicated as potent lipid mediators of various biological processes. Enzymatic formations of eicosanoids are regioselective and enantioselective, whereas reactive oxygen species (ROS)-mediated formation proceeds with no stereo-selectivity. To distinguish between enzymatic and non-enzymatic pathways of eicosanoid formation, it is necessary to resolve enantiomeric forms as well as regioisomers. High sensitivity is also required to analyze the eicosanoid lipids that are usually present as trace amounts (pM level) in biological fluids. A discovery of liquid chromatography-electron capture atmospheric pressure chemical ionization/mass spectrometry (LC-ECAPCI/MS) allows us to couple normal phase chiral chromatography without loss of sensitivity. Analytical specificity was obtained by the use of collision-induced dissociation (CID) and tandem MS (MS/MS). With combination of stable isotope dilution methodology, complex mixtures of regioisomeric and enantiomeric eicosanoids have been resolved and quantified in biological samples with high sensitivity and specificity. Targeted chiral lipidomics profiles of bioactive eicosanoid lipids obtained from various cell systems and their biological implications have been discussed.

Mass Spectrometer를 이용한 대두 배아 출추 Cerebroside의 구조 분석 (Structural Determination of Cerebrosides from Soybean Embryo by Mass Spectrometer)

  • 김정훈;장석윤;김여경
    • 분석과학
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    • 제6권3호
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    • pp.335-343
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    • 1993
  • Fast atom bombardment mass spectrometer(FAB-MS), gas chromatography mass spectrometer(GC-MS), TLC 등을 이용하여 대두 배아 추출 cerebroside의 구조를 분석하였다. Cerebroside를 이루고 있는 각각의 구성 성분은 화학적인 산분해 후 GC-MS로 분석하였다. Cerebroside의 분자량 분포는 LiOH로 포화된 3-nitrobenzyl alcohol(3-NBA)를 matrix로 한 양이온 검출 FAB-MS법으로 측정하였다. FAB-MS와 GC-MS 결과를 종합하여 cerebroside의 구조를 해석함으로써 기존의 분석법이 가지고 있던 문제점을 개선하였다. 대두 배아로부터 추출한 cerebroside의 대부분은 N-2'-hydroxy palmitoyl-sphingadienine에 당이 한 분자 결합된 형태로 존재하였으며 그 조성이 매우 단순하였다.

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