• 제목/요약/키워드: h2 Separation

검색결과 1,281건 처리시간 0.032초

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.

한국산 물통이속(Pilea) 식물의 nrDNA, cpDNA를 통한 계통분석 (A phylogenetic analysis of the genus Pilea (Urticaceae) using nrDNA and cpDNA sequences)

  • 문애라;박정미;장창기
    • 식물분류학회지
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    • 제45권2호
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    • pp.158-168
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    • 2015
  • 한국산 물통이(Pilea)속 식물의 분자계통학적 연구를 통해서 총 1속 5분류군으로 정리하였다. 물통이속은 모두 1년생 초본으로, 그늘지고 습기가 있는 지역에서 서식하며, 여름에 꽃이 피고, 가을에 열매를 맺는다. nrDNA의 ITS regions과 cpDNA의 psbA-trnH regions의 DNA 염기서열의 분석 결과, 산물통이, 물통이는 분계조를 각각 형성하였다. 하지만 제주 산방산의 제주큰물통이는 내륙지역의 지리산에서 자생하는 제주큰물통이와 같은 분계조를 형성하지 못하고 큰물통이, 모시물통이와 섞여 분계조를 형성하였다. ITS1, 4 regions에서만 DNA 염기서열이 분석된 지리산의 제주큰물통이 역시 완전히 다른 분계조를 형성하였다. 단순히 지리적인 차이로 인해 형성되었다고 보기에 무리가 있을 것으로 생각되어지며, 후에 좀 더 많은 연구가 이루어져야 할 것으로 생각되어진다.

새로운 이온용액의 제조 및 브롬화반응 응용 (Preparation of Novel Ionic Liquids and Their Applications in Brominating Reaction)

  • Li, Hua;Liu, Juan;Zhu, Jiang;Wang, Hongkai
    • 대한화학회지
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    • 제55권4호
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    • pp.685-690
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    • 2011
  • 새로운 산성 이온용액인1-(${\omega}$-sulfonicacid)propyl-3-methylimidazolium bromide ([$HSO_3$pmim]Br)과 1-(${\omega}$-sulfonicacid)-butyl-3-methylimidazolium bromide([$HSO_3$bmim]Br)을 제조하였다. 이 화합물들을 브롬화 시약 및 용매로 사용하여 $100^{\circ}C$, 2시간 반응시켰으며, 간단히 상분리에 의해 1,7-dibromoheptane을 95% 수율로 합성하였다. 이 산성 이온용액을 5회 재사용하였으나 수율 감소가 관찰되지 않았다.

Methacrylamidohistidine in Affinity Ligands for Immobilized Metal-ion Affinity Chromatography of Human Serum Albumin

  • Odaba, Mehmet;Garipacan, Bora;Dede, Semir;Denizli, Adil
    • Biotechnology and Bioprocess Engineering:BBE
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    • 제6권6호
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    • pp.402-409
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    • 2001
  • Different bioligands carrying synthetic adsorbents have been reported in the literature for protein separation, We have developed a novel and new approach to obtain high protein ad-sorption capacity utilizing 2-methacrylamidohistidine(MAH) as a bioligand. MAH was synthe-sized by reacting methacrylocholride and histidine, Spherical beads with an average size of 150-200㎛ were obtained by the radical suspension polymerization of MAH and 2-hydrosyethyl-methacrylate(HEMA) conducted in an aqueous dispersion medium. p(HEMA-co-MAH) beads had a specific surface area of 17.6㎡/g . Synthesized MAH monomer was characterized by NMR. p(HEMA-co-MAH) beads were characterized by swelling test, FTIR and elemental analysis. Then Cu(II) ions were incorporated onto the beads and Cu(II) loading was found to be 0.96 mmol/g.These affinity beads with a swelling ration of 65% and containing, 1.6 mmol MAH/g were used in the adsorption/desorption of human serum albumin(HSA) from both aqueous solutions and hu-man serum. The adsorption of HSA onto p(HEM-co-MAH) was low(8.8 mg/g). Cu(II) chelation onto the beads significantly increased the HSA adsorption (56.3 mg/g). The maximum HSA ad-sorption ws observed at pH 8.0 Higher HSA adsorption was observed from human plasma(94.6 mgHSA/g) Adsorption of other serum proteins were obtained as 3.7 mg/g for fibrinogen and 8.5mg/g for γ-globulin. The total protein adsorption was determined as 107.1mg/g. Desorption of HSA was obtained using 0.1 M Tris/HCl buffer containing 0.5 M NaSCN, High desorption rations(up to 98% of the adsorbed HSA) were observed. It was possible to reuse Cu(II) chelated-p(HEMA-co-MAH) beads without significant decreases in the adsorption capacities.

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Structural Characterization of Physiologically Active Polysaccharides from Natural Products (Arabidopsis)

  • Shin, Kwang-Soon;Darvill, Alan G.
    • Food Science and Biotechnology
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    • 제15권3호
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    • pp.447-452
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    • 2006
  • To determine the functions of specific cell wall polysaccharides, polysaccharides of three mutants, mur3-1, mur3-2, and mur3-3, obtained from Arabidopsis wild type, underwent structural characterization. Upon sequential separation of pectins (RG-I and RG-II) and cross-linking glycans (xyloglucan, XG), only XG was affected by the mud mutation. Wild-type XG contained a considerable amount of fucose, whereas the fucose level in mur3 XGs was less than 20% that of wild type. Further analysis of XGs by matrix-assisted laser-induced/ionization time-of-flight (MALDI-TOF) mass spectrometry indicated that mud lines considerably or completely lost the fucosylated XG oligosaccharides such as XXFG and XLFG and the double-galactosylated oligosaccharide XLLG $^1H$-NMR spectroscopic analyses of the XG oligosaccharides from mur3-3 plant revealed the absence of fucose and a galactose level in the galactosylated side chain that was reduced by 40% compared to that of Arabidopsis wild-type plant. In contrast, 85% less fucose and a slight loss of galactose were observed in the mur3-1 and mur3-2 lines which show normal growth habit. Of the three Arabidopsis mur3 lines studied here, mur3-3 is disrupted by a T-DNA insertion in the exon of MUR3 which encodes XG-specific galactosyltransferase, and exhibits slight dwarfism. These results indicated that the T-DNA insertion at the MUR3 locus did not induce the complete loss of galactose in XG, and that galactose, rather than fucose, in the XG side chains made a major contribution to overall wall strength.

Determination of Bergenin in Different Parts of Bergenia ciliata using a Validated RP-HPLC Method

  • Ali, Ejaz;Hussain, Khalid;Bukhari, Nadeem Irfan;Arshad, Najma;Hussain, Amjad;Abbas, Nasir;Arshad, Sohail;Parveen, Sajida;Shehzadi, Naureen;Qamar, Shaista;Qamar, Abida
    • Natural Product Sciences
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    • 제27권1호
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    • pp.54-59
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    • 2021
  • Bergenia ciliata (Family: Saxifragaceae) is a folklore remedy for the treatment of various ailments in Asian countries. Bergenin (1) has been isolated as an active constituent in many studies, however, the amount of bergenin has not been determined in all parts of the plant. A simple RP-HPLC method was developed to determine the amount of bergenin in methanol extracts of leaves, rhizomes and roots of the plant. Separation was achieved on an Agilent Eclipse XDB-C18 column maintained at 25 ℃ using isocratic solvent system (water: methanol: acetic acid; 62.5:37:0.5 v/v/v) adjusted at pH 2 0 at a flow rate of 1.0 mL/min. and detected at 275 nm. Correlation coefficient (0.9952) showed linearity of concentration (5-200 ㎍/mL) and response. The values of LOD (0.00947 ㎍/mL) and LOQ (0.02869 ㎍/mL) indicated that method was sensitive. The recovery of bergenin was 99.99-100% indicating accuracy of method. The methanol extract of rhizomes contained higher amount of bergenin (19.4%) than roots (9.2%) and leaves (6.9%). It is concluded that methanol extract of rhizomes is a better source of bergenin than other parts of the plant. The findings are useful for standardization of bergenin containing extracts and herbal preparations.

Nondestructive Determination of Sugar Contents in Shingo Pears with Different Temperature

  • Lee, Kang-J.;Choi, Kyu H.
    • 한국근적외분광분석학회:학술대회논문집
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    • 한국근적외분광분석학회 2001년도 NIR-2001
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    • pp.1264-1264
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    • 2001
  • The affect of surface temperatures of fruits on spectrum which measures actual sugar contents was observed. PLSR was applied to develop the sugar content evaluation system that was not affected by temperature. The reflected spectrum was used at the wavelengths of 654 and 1052nm with the separation distance of 2.5nm. To increase the conformance of a model using unknown samples, let the minimum value of PRESS be an optimum factor. 71 Shingo pears stored in a refrigerator were left in a room temperature for a while and these temperatures and reflected spectrums were measured. Reflected spectrums were measured at the wavelengths of 654 and 1052nm, 3 samples in one second. To measure these at different temperatures, the experiment was repeated hourly and four times. Starting temperatures of 2-3 were increased up to 17. The total number of measured spectrum was 284. To develop a sugar content evaluation system model using measured reflected spectrum, three groups of samples were considered. First group had 51 samples at 14 and second group had 141 samples with lower or higher temperatures than 14. Third group had 155 samples with well distributed temperatures. Other samples were used as validations to ensure the conformance. Measuring the sugar contents of samples with surface temperatures other than 14 were difficult with PLS model I, developed by using a sample temperature of 14. If the sugar contents were compensated using samples' temperatures, results of prediction would be close to the expected results and it would be one of the most important factors to develop this system. PLS models I and II could compensate the temperature but the precision would not come up to the standard. High precision was expected by using samples with wide ranges of temperatures and sugar contents. Both models showed the possibility of an improvement of a sugar content evaluation system disregarding the temperature. For practical use of a system, selecting samples should be done carefully to reduce the effect of the temperature.

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Effect of post-treatment routes on the performance of PVDF-TEOS hollow fiber membranes

  • Shadia R. Tewfik;Mohamed H. Sorour;Hayam F. Shaalan;Heba A. Hani;Abdelghani G. Abulnour;Marwa M. El Sayed;Yomna O. Mostafa;Mahmoud A. Eltoukhy
    • Membrane and Water Treatment
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    • 제14권2호
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    • pp.85-93
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    • 2023
  • Membrane separation is widely used for several applications such as water treatment, membrane reactors and climate change. Cross-linked organic-inorganic hybrid polyvinylidene fluoride (PVDF) / Tetraethyl orthosilicate (TEOS) was adopted for the preparation of optimized hollow membrane (HFM) for membrane distillation or other low pressure separators for mechanical properties and permeability under varying pretreatment schemes. HFMs were prepared on semi-pilot membrane fabrication system. Novel adopted post-treatment schemes involved soaking in glycerol, magnesium sulphate (MgSO4), sodium hypochlorite (NaOCl), and isopropanol for different durations. All fibers were characterized for morphology using a scanning electron microscope (SEM), surface roughness using atomic force microscope (AFM), elemental composition by examining Energy Dispersive Spectroscopy (EDS), water contact angle (CA°) and porosity. The performance of the fibers was evaluated for pure water permeation flux (PWF). Post-treatment with MgSO4 gave the highest both tensile modulus and flux. Assessment of properties and performance revealed comparable results with other organic-inorganic separators, HF or flat. In spite of few reported data on post treatment using MgSO4 in presence of TEOS, this proves the potential of low cost treatment without negative impact on other membrane properties. The flux is also comparable with hypochlorite which manifests substantial precaution requirements in actual industrial use.The relatively high values of flux/bar for sample treated with TEOS, post treated with MgSO4 and hypochlorite are 88 and 82 LMH/bar respectively.

입상 활성탄에 대한 비스마르크 브라운 R 염료의 흡착평형, 동력학 및 열역학 파라미터에 관한 연구 (Adsorption Equilibrium, Kinetics and Thermodynamic Parameters Studies of Bismarck Brown R Dye Adsorption on Granular Activated Carbon)

  • 이종집
    • 공업화학
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    • 제24권3호
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    • pp.327-332
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    • 2013
  • 입상 활성탄에 대한 bismarck brown R의 흡착평형, 동력학 및 열역학 파라미터들을 회분식 실험을 통해 살펴보았다. 조작변수로서 초기농도, 접촉시간과 흡착온도의 영향을 조사하였다. 흡착평형자료는 선형회귀법을 사용하여 Langmuir와 Freundlich 흡착등온식에 대한 적합성을 평가하였다. 흡착평형은 Freundlich 흡착등온식이 더 잘 맞았으며, 계산된 분리계수(1/n) 값으로부터 입상 활성탄이 bismarck brown R을 효과적으로 처리할 수 있다는 것을 알 수 있었다. 동력학적 실험으로부터, 흡착공정은 유사이차반응속도식에 잘 맞으며, 속도상수($k_2$) 값은 온도가 증가할수록 증가하였다. 활성화에너지, 엔탈피, 엔트로피 및 Gibbs 자유에너지변화와 같은 열역학 파라미터들은 흡착공정의 특성을 평가하기 위하여 298~318 K의 온도 범위에서 조사하였다. 활성화 에너지의 계산값은 100 mg/L에서 8.73 kJ/mol로 입상 활성탄에 대한 bismarck brown R의 흡착이 물리적 공정임을 나타냈다. Gibbs 자유에너지변화의 음수값(${\Delta}G$ = -2.59~-4.92 kJ/mol)과 엔탈피변화의 양수값(${\Delta}H$ = +26.34 kJ/mol)은 흡착공정이 자발적이며 흡열과정으로 일어난다는 것을 나타냈다.

Shell 석탄가스화 복합발전 시스템의 성능해석 연구 (Performance Analysis of Shell Coal Gasification Combined Cycle systems)

  • Kim, Jong-Jin;Park, Moung-Ho;Song, Kyu-So;Cho, Sang-Ki;Seo, Seok-Bin;Kim, Chong-Young
    • 에너지공학
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    • 제6권1호
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    • pp.104-113
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    • 1997
  • 본 연구에서는 상용공정모사기인 ASPEN PLUS를 이용하여 건식탄공급, 산소사용 분류층 가스화기인 Shell가스화공정, 저온가스정제공정, GE MS7001FA가스터빈, 삼압.자연순환식 폐열회수보일러, 재열복수식 증기터빈 및 극저온 산소분리공정을 채용한 IGCC시스템에 대하여 성능해석 모델을 개발하고 시스템 성능해석을 위한 민감도분석을 수행하였다. 본 모델의 적정성은 설계조건에서 대상탄을 이용한 정상상태 성능해석 결과를 타 시뮬레이션 결과와 비교함으로서 검증하였다.$^{1)}$ . Illinois#6탄을 대상으로 수행한 시뮬레이션 결과는 투입되는 탄에 함유된 수분의 양이 증가함에 따라 가스화기의 온도가 감소하며, 회분 및 황이 많은 경우에 현열손실이 증가하여 시스템 효율이 감소하였다. 개발된 모델을 이용하여 가스화기의 운전압력, 증기/석탄비율 및 산소/석탄비율에 따르는 시스템의 민감도분석을 수행한 결과 운전압력 증가에 따라 가스화기 노내온도가 상승하며, 가연성가스(CO+H2) 생성율이 감소하였다. 증기/석탄비율 변화분석에서는 공급증기의 양을 변화시키면 가연성가스의 최고생성점이 보다 낮은 산소/석탄비율에서 나타남을 알 수 있었다. 또한 산소/석탄비율 변화분석에서는 증기/석탄 공급비율 0.2에서 산소/석탄 공급비율이 0.77인 경우에 가장 최적의 운전조건임을 알 수 있었다.

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