• 제목/요약/키워드: Chiral Separation

검색결과 194건 처리시간 0.029초

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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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.

Kromasil HPLC 칼럼에서 Mandelic Acid의 분리특성 (Separation Characteristics of Mandelic Acid in Kromasil HPLC Column)

  • 김병립;김종민;김우식;김인호
    • Korean Chemical Engineering Research
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    • 제46권4호
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    • pp.681-685
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    • 2008
  • Kromasil KR100-5CHI-TBB 칼럼을 사용하여 라세미 mandelic acid를 분리하였다. 분리도(resolution), 이론단수(number of theoretical plates), 용량인자(capacity factor)와 같은 크로마토그라피 변수들을 이동상의 조성(hexane/t-BME = 85/15 - 10/90)과 포름산 농도(0.1, 0.5, 1.0 v/v%)를 변화시켜 실험하여 계산하였다. 칼럼의 효율을 평가하기 위해 유속 대 이론단수를 비교하였다. 등온흡착식을 계산하기 위해 PIM(Pulse Input Method)을 사용하였고, mandelic acid의 농도가 0.1에서 0.3 mg/ml 사이일 때 L-과 D-mandelic acid가 각각 8.8분과 9.4분의 체류시간을 보였다. Mandelic acid의 등온흡착식은 0.3 mg/ml의 농도이하와 이동상 조성(hexane/t-BME = 75/25)에서 선형이었다. Mandelic acid의 농도가 증가할수록 mandelic acid는 비선형 거동을 보였고, Langmuir 등온흡착식은 L-과 D-mandelic acid의 경우 각각 $C_{S,L}=3.358C_{M,L}/(1+0.0897C_{M,L})$, $C_{S,D}=3.692C_{M,D}/(1+0.1457C_{M,D})$이었다.

Enantiospecific separation in biphasic Membrane Reactors

  • Giorno, Lidietta
    • 한국막학회:학술대회논문집
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    • 한국막학회 1998년도 추계 총회 및 학술발표회
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    • pp.15-18
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    • 1998
  • Membrane reactors are systems which combine a chemical reactor with a membrane separation process allowing to carry out simultaneously conversion and product separation. The catalyst can be immobilized on the membrane or simply compartmentalized in a reaction space by the membrane. Membrane reactors are today investigated to produce optically pure isomers and/or resolve racemic mixture of enantiomers. The interest towards these systems is due to the increasing demand of enantiomerically pure compounds to be used in the pharmaceutical, food, and agrochemical industries. In fact, enantiomers can have different biological activities, which often influence the efficacy or toxicity of the compound. On the basis of current literature there are basically two schemes on the use of membrane technology to produce enantiomers. In one case, the membrane itseft is intrinsically enantioselective: the membrane is the chiral system which selectively separates the wanted isomer on the basis of its conformation. In the other, a kinetic resolution using an enantiospecific biocatalyst is combined with a membrane separation process; the membrane separates the product from the substrate on the basis of their relative chemical properties (i.e. solubility). This kind of configuration is widely used to carry out kinetic resolutions of low water soluble substrams in biphasic membrane reactors [Giomo, 1995, 1997; Lopez, 1997]. These are systems where enzyme-loaded membranes promote reactions between two separate phases thanks to the properties of enzymes, such as lipases, to catalyse reactions at the org ic/aqueous interface; the two phases are maintained in contact and separated at the membrane level by operating at appropriate transmembrane pressure. A schematic representation of biphasic membrane reactor is shown in figure 1, while an example of enantiospecific reaction and product separation carried out with these systems is reported in figure 2.

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키랄킬레이트 이동상첨가법에 의한 답실아미노산의 광학이성질체 분리 (Optical Resolution of DABS-Amino Acids with Mobile Chiral Chelate Addition)

  • 이선행;오대섭;변성구
    • 대한화학회지
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    • 제34권4호
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    • pp.345-351
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    • 1990
  • 역상 고성능 액체 크로마토그래피에 Cu (Ⅱ)-L-Proline 킬레이트를 이동상에 첨가하여 답실아미노산(DABS-AA)을 광학분리했다. DABS-아미노산에 관한 머무름거동을 이동상으로 아세토니트릴, 착물 및 완충용액의 농도와 pH에 따라 연구 검토했다. DABS-아미노산의 광학분리선택성은 이동상의 pH와 킬레이트의 농도가 증가하면 증가하나 유기용매의 농도에 따라 감소한다. 완충액의 농도에는 무관하다. DABS-아미노산과 구리 착물간의 리간드 교환반응의 입체효과에 따른 시스-트란스 생성으로 분리메카니즘을 설명할 수 있다.

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SMB 크로마토그래피를 이용한 loxoprofen racemate의 분리

  • 윤태호;김인호
    • 한국생물공학회:학술대회논문집
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    • 한국생물공학회 2003년도 생물공학의 동향(XIII)
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    • pp.549-553
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    • 2003
  • TMB 크로마토그래피의 물질수지식으로부터 SMB 크로마토그래피의 디자인 파라미터들을 계산할 수 있으며, 이를 이용하여 6 칼럼 SMB 크로마토그래피 장치를 디자인하였다. SMB 크로마토그래피 장치는 4개의 multi position rotary valve를 사용하여 연속적으로 각 칼럼으로의 유로를 제어할 수 있으며, 효율적인 SMB 크로마토그래피 장치를 구현할 수 있다. 또한 회분식 실험으로부터 얻어진 $m_2,$ $m_3$ diagram으로부터 SMB 크로마토그래피의 조작에 필요한 파라미터들을 계산할 수 있었다.

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SS-epm이 배위된 trans-dichlorocobalt(III) 착물과 라세미 propane-1,2-diamine과의 입체선택적 리간드 치환반응 (Stereoselective Ligand Exchange Reaction of trans-dichlorocobalt(III) complex contained SS-epm and racemi propane-1,2-diamine)

  • 김동엽
    • 한국산업융합학회 논문집
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    • 제3권1호
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    • pp.77-82
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    • 2000
  • The stereoselective ligand exchange reaction of trans-$[Co(SS-epm)Cl_2]^+$ and racemic propane-1,2-diamine (rac-pn) produces the complex that is identified as $[CO(N)_6]^{3+}$ type of $[Co(SS-epm)(pn)]^{3+}$ by absorption spectrum. It is conceivable that the reaction mechanism involves substitution and isomerization. The calculated and experimentally determined ratios of the complexed enantiomeric substrates at equilibrium were as follows: $[Co(SS-epm)(pn)]^{3+}$,calcd 32 % / 68 %, exptl 19 % / 81 % R-pn / S-pn. It has been shown that the employment of molecular mechanics calculations as a predictive tool may lead to the design of chiral complexes that may be applied to the separation of racemic mixtures of simple bidentate ligands.

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포지용 오프셋 PS판의 현상액 개발 (A Study on the development of developer for positive type presensitized off-set plates)

  • 오세웅
    • 한국인쇄학회지
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    • 제16권1호
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    • pp.1-11
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    • 1998
  • Recently the study of the application of liquid crystal in industrial fields has developed rapidly. It is well known that the encapsulated liquid crystal is advantageous than raw liquid crystal for protection of surface pollution. This paper describes a new class of thermal sensor. It is that the liquid crystal polymer composite(LCPC) films consisting of a continuous LC phase embedded in a three-dimensional network of polymer matrix are formed by photopolymerization-induced phase separation. In this works, it has been demonstrated that consiste of a 8:2 mixture of chiral nematic liquid crystal and HX-620 has the greatest domain and it was best discoloration.

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Optical Purity Determination of (S)-Ibuprofen in Tablets by Achiral Gas Chromatography

  • Paik, Man-Jeong;Kim, Kyoung-Rae
    • Archives of Pharmacal Research
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    • 제27권8호
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    • pp.820-824
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    • 2004
  • An optical purity test was indirectly performed on (S)-ibuprofen as its diastereomeric (R)-(+)-1-phenylethylamide derivative using achiral gas chromatography (GC). The method for the determination of trace (R)-ibuprofen (optical impurity), within the range 1.0 to 50 ng, from a racemic ibuprofen standard was linear (r=0.9997) with acceptable precision (% $RSD{\leq}5.3$) and accuracy (% RE=0.7~-3.9). Similar results were obtained with the method validation for the quantification of (S)-ibuprofen within the range 0.1 to 2.0 $\mu\textrm{g}$ using a (S)-ibuprofen stan-dard. When applied to seven different commercial (S)-ibuprofen products, their optical purities (98.7~99.1%) were determined with good precision (% $RSD{\leq}4.0$).