• 제목/요약/키워드: chiral analysis

검색결과 88건 처리시간 0.02초

Chiral separation of amino acids in urine specimens from patients with inherited metabolic disorders by achiral gas chromatography

  • Paik, Man-Jeoneg;Choi, Young-Mie;Nguyen, Duc-Toan;Kim, Ji-Yung;Kim, Jung-Han;Kim, Kyoung-Rae
    • 대한약학회:학술대회논문집
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    • 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2-2
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    • pp.218.2-218.2
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    • 2003
  • An efficient method is described for the enantioseparation of urinary amino acids to determine their absolute configurations. It involves two-phase extractive ethoxycarbonylation in alkaline aqueous solution with subsequent extraction after acidification. The resulting derivatives of amino acids are converted to volatile diastereomeric esters or amides for the direct analysis by gas chromatography (GC) on achiral dual-columns with different polarities. The present method was applied to urine specimens from patients with inherited metabolic disorders. In this study, the usefulness for the chiral separation of diagnostic amino acids will be discussed.

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Recommendation for the modelling of Donnell shell: The relationship between non-local parameter and frequency

  • Mohamed A. Khadimallah;Muzamal Hussain;Elimam Ali;Sehar Asghar;Abdelouhed Tounsi
    • Computers and Concrete
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    • 제32권2호
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    • pp.165-172
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    • 2023
  • The vibration analysis of armchair, zigzag and chiral double-walled carbon nanotubes has been developed by inserting the nonlocal theory of elasticity into thin shell theory. First Donnell shell theory is employed while exercising wave propagation approach. Scale effects are realized by using different values of nonlocal parameters under certain boundary conditions. The natural frequencies have been investigated and displayed for various non-local parameters. It is noticed that on increasing nonlocal parameter, the frequency curve tends to decrease. The frequency estimates of clamped-free boundary condition are less than those of clamped-clamped and simply supported computations. The frequency comparisons are presented for armchair, zigzag and chiral nanotubes. The software MATLAB is used to extract the frequencies of double walled carbon nanotubes.

Multidimensional Gas Chromatography-A Powerful Tool for the Analysis of Multicomponent Mixtures

  • Kim, Kyoung-Su
    • Preventive Nutrition and Food Science
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    • 제1권1호
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    • pp.127-133
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    • 1996
  • The development of high resolution capillary columns and a large variety of different detectors led to a strong position of gas chromatography in instrumental analysis. Every effort has been made to solve sophisticated separation problems by column switching. Nowadays, several systems are commercially available for this purpose. The principle and the capabilities of multidimensional gas chromatography(MDGC) are illustrated by different applications in the field of modern flavor and essential oil research.

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알루미나 나노산화물이 Nitrendipine 제조 공정에 미치는 영향 (Effect of Alumina Nanooxide Application on Nitrendipine Manufacturing Process)

  • 채은진;엄영랑;한병선;이창규;박상언
    • 한국분말재료학회지
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    • 제14권2호
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    • pp.127-131
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    • 2007
  • The alumina nano powders synthesized by levitational gas condensation (LGC) method were applied to catalyst in manufacturing process of Hanzsch reaction for Nitrendipine. The L-tartaric acid on the surface is carried out with participation of carbonyl fragments, O-H, C-H bonds which affects stereo selectivity, yield on the reagents positively. From the analysis of the IR-spectroscopy, the carbonyl fragments, O-H, and C-H bond were created by the catalytic reaction. From the analysis of the rR-spectroscopy, the carbonyl fragments, O-H, and C-H bond were created by the catalytic reaction. The newly created bonds made a chiral center on the final product.

Structure Identification of 1,2-Disubstituted Chiral Calix[4]arene : X-Ray and NMR Analysis of 25-(3,5-Dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene

  • 박영자;신정미;남계춘;김종민;국승근
    • Bulletin of the Korean Chemical Society
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    • 제17권7호
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    • pp.643-647
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    • 1996
  • 1,2-Disubstituted chiral calix[4]arene "25-(3,5-dinitrobenzoyloxy)-26-methoxy-27,28-dihydroxycalix[4]arene" was synthesized by the reaction of 25-(3,5-dinitrobenzoyloxy)-calix[4]arene with methyl iodide in the presence of K2CO3. Methylation was occurred at the 26-position of calix[4]arene. The partial cone conformation and 1,2-substitution were characterized based on the 1H NMR, 13C NMR and X-ray diffraction analysis. The crystal structure has been determined by X-ray diffraction method. The crystals are orthorhombic, Pbca, a=10.652(1), b=17.687(1), c=32.247(3) Å, Z=8, V=6075.4(9) Å3, Dc=1.38gcm-3. The intensity data were collected on an Enraf-Nonius CAD-4 Diffractometer with a graphite monochromated Cu-Kα radiation. The structure was solved by direct method and refined by full-matrix least-squares methods to a final R value of 0.050 for 2368 observed reflections. The molecule is in the partial cone conformation. It has two strong intramolecular hydrogen bonds of O(1D)-H…O(1C)-H…O(1B).

폴리머 키랄 살렌을 함유한 메조세공 모더나이트의 비대칭 촉매 활성 (Asymmetric Catalytic Activity of Mesoporous Mordenite containing Polymeric Chiral Salen Complexes in the Mesopore System)

  • 곽소봉;김용석;라울;김건중
    • 공업화학
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    • 제20권3호
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    • pp.279-284
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    • 2009
  • 모더나이트결정 중의 실리카를 제어된 알칼리용액의 처리로 추출제거하여 중간세공이 형성되도록 하였다. 형성된 중간세공의 크기는 알칼리용액의 농도를 변화시킴으로써 조절할 수 있었다. 알칼리처리 후의 모더나이트 제올라이트 내부의 세공구조를 조사하였다. 새둥지형태의 중간세공을 형성시키기 위해서는, 알칼리용액 처리전에 모더나이트결정의 바깥표면을 티타니아로 코팅하는 것이 가장 효과적임을 관찰하였다. 모더나이트 내부의 중간세공에 고분자형의 코발트(III) 살렌착체를 "ship-in-a-bottle"법으로 가둔 촉매를 제조하였다. 이 고정화촉매를 물에 의한 에피클로로히드린의 산소고리열림반응에 사용하여, 촉매반응에서 높은 수율과 광학선택성을 얻을 수 있었다.

Determination of nadolol enantiomers in human plasma using a coupled achiral-chiral high-performance liquid chromatography method

  • Lee, Seung-Beom;Pham, Thuy-Vy;Mai, Xuan-Lan;Le, Thi-Anh-Tuyet;Nguyen, Thi-Ngoc-Van;Kang, Jong-Seong;Mar, Woongchon;Kim, Kyeong Ho
    • 분석과학
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    • 제33권2호
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    • pp.59-67
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    • 2020
  • Nadolol is a β-blocker drug, which effectively manages hypertension and angina pectoris. Its chemical structure allows the formation of four possible stereoisomers. A coupled column high-performance liquid chromatographic (HPLC) system with UV and fluorescence detection was investigated for simultaneously determining four nadolol enantiomers in human plasma. The plasma samples were prepared using a convenient liquid-liquid extraction process and passed through HPLC. Nadolol was initially separated from the endogenous compounds or other impurities in human plasma on a Phenomenex silica column, and its enantiomers were resolved and determined on a Chirapak AD-H column. The developed HPLC method achieved an effective chiral separation and significantly eliminated endogenous compound interference. This optimal HPLC method was validated following FDA guidelines. The results showed good selectivity, linearity, accuracy (90.50 % - 105.27 %), and precision (RSDs < 9.52 %) for each enantiomer. This method was also successfully applied to determine nadolol enantiomers in the plasma samples of a healthy male volunteer (after orally administering 80 mg racemic nadolol), proving its suitability for nadolol stereoselective pharmacokinetic studies.

무세포 단백질합성 시스템 기반의 epoxide hydrolase 발현 및 활성 분석 (Assay of Epoxide Hydrolase Activity Based on PCR-linked in vitro Coupled Transcription and Translation System.)

  • 이옥경;김희숙;이은열
    • 생명과학회지
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    • 제15권5호
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    • pp.779-782
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    • 2005
  • Coupled transcription/translation cocktail을 이용하여 R. glutinis EH 유전자를 in vitro에서 합성하고 활성을 평가하였다. SDS-PAGE 및 immunoblotting을 통하여 45 kDa 크기의 EH 단백질이 발현되었음을 확인하였고, NBP assay 및 chiral GC 분석을 통해 발현된 단백질이 (R)-styrene oxide에 대한 입체선택성이 있음을 확인하였다. 따라서 무세포 단백질 합성 시스템을 이용하여 입체선택성을 유지시킨 EH 유전자 발현이 가능하며, 이러한 방법은 putative EH 유전자 탐색 등에 효율적으로 응용될 것이다.

D체와 R체 이성질체 판별과 GC-MS를 이용한 유전성 대사이상질환의 진단법 개발 (Diagnostic Method for Inborn Metabolic Disorders using differentiation between D- and R- Isomers on GC-MS)

  • 윤혜란
    • 대한유전성대사질환학회지
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    • 제15권2호
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    • pp.65-71
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    • 2015
  • Since the secretion of specific chiral isomers in urine (or plasma) is very crucial to diagnose some inborn metabolic disorders, clinical application of dual column achiral differential method has been performed for the absolute configuration of chiral compounds. Extracted from the acidified urine with diethyl ether, carboxylic functional group of organic acid (stereoisomers of the volatile) was derivatized with (-)-menthylation or (S)-(+)-3-methyl-2-butylation and followed by O-trifluoroacylation. Each of the enantiomers was accurately separated from the library matched double column (achiral) with a retention index (I). In various inborn metabolic disease urines, absolute chirality was identified correctly in the urine (10 patients) with inborn metabolic disease (including secretion of D, L- lactic acid, D, L-3-hydroxybutyric acid, and D, L-2-hydroxyglutaric acid). In this study, we identified and isolated the volatile diastereomer as a useful diagnostic marker, this successful application to urine specimens may be useful for diagnostic classification of inherited metabolic disorders.

Effect of chiral structure for free vibration of DWCNTs: Modal analysis

  • Asghar, Sehar;Naeem, Muhammad N.;Khadimallah, Mohamed Amine;Hussain, Muzamal;Iqbal, Zafar;Tounsi, Abdelouahed
    • Advances in concrete construction
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    • 제9권6호
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    • pp.577-588
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    • 2020
  • In this paper, vibration attributes of chiral double-walled carbon nanotubes (CNTs) based on nonlocal elastic shell model have been investigated. The impact of small scale is being perceived by establishing Flügge shell model. The wave propagation is engaged to frame the ruling equations as eigen value system. The influence of nonlocal parameter subjected to different end supports has been overtly examined. A suitable choice of material properties and nonlocal parameter been focused to analyze the vibration characteristics. The new set of inner and outer tubes radii investigated in detail against aspect ratio and length. The dominance of boundary conditions via nonlocal parameter is shown graphically. Whereas for lower aspect ratio the frequencies coincide but as it continues to expand the difference between all respective boundary conditions slightly tend to increase. The results generated furnish the evidence regarding applicability of nonlocal shell model and also verified by earlier published literature.