• Title/Summary/Keyword: Aqueous Phase

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Liquid Chromatographic Resolution of Tocainide and Its Analogues on a Doubly Tethered Chiral Stationary Phase Based on (+)-(18-Crown-6)-2,3,11,12-tetracarboxylic Acid

  • Kim, Hee-Jin;Choi, Hee-Jung;Hyun, Myung-Ho
    • Bulletin of the Korean Chemical Society
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    • v.31 no.3
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    • pp.678-682
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    • 2010
  • A doubly tethered chiral stationary phase (CSP) based on (+)-(18-crown-6)-2,3,11,12-tetracarboxylic acid were applied to the liquid chromatographic resolution of racemic tocainide, an antiarrhythmic agent, and its analogues. The chiral recognition efficiency of the doubly tethered CSP for tocainide and its analogues was generally greater than that of the corresponding singly tethered CSP especially in terms of the resolution ($R_S$). The resolution of tocainide and its analogues on the doubly tethered CSP were dependent on the content and the type of the organic and acidic modifiers in aqueous mobile phase and the column temperature. Especially, the retention behaviors of analytes on the doubly tethered CSP with the variation of the content of organic modifier in aqueous mobile phase were opposite to those on the corresponding singly tethered CSP and these opposite retention behaviors were rationalized by the lipophilicity differences of the two CSPs.

Removal Characteristics of Cu(II) by Solid Phase Extractant Immobilized with D2EHPA and TBP in Styrene Acrylonitrile Copolymer (SAN) (D2EHPA와 TBP를 Styrene Acrylonitrile Copolymer (SAN)으로 고정화한 고체상 추출제에 의한 Cu(II) 제거 특성)

  • Kam, Sang-Kyu;Lee, Min-Gyu
    • Journal of Environmental Science International
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    • v.24 no.7
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    • pp.841-849
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    • 2015
  • The solid phase extractant SAN-D2EHPA/TBP containing two extractants of Di-(2-ethylhexyl)phosphoric acid (D2EHPA) and Tri-butyl-phosphate (TBP) was prepared by immobilizing two exractants D2EHPA and TBP in styrene acrylonitrile copolymer (SAN). The prepared SAN-D2EHPA/TBP was characterized by using fourier transform infrared spectrometer (FTIR) and scanning electron microscopy (SEM). The solid phase extractant SAN-D2EHPA/TBP was tested for the removal of Cu(II) from aqueous solution. Experiments were carried out as a function of the pH and Cu(II) concentration in the aqueous phase. The equilibrium time was 180 min and equilibrium experiment data obeyed the pseudo-second-order kinetic model. The Langmuir isotherm model represented the experiment data as well. The maximum removal capacity of Cu(II) calculated from Langmuir isotherm model was 3.1 mg/g.

Synthesis of Nanosized Brookite-type Titanium Dioxide Powder from aqueous TiOCl2 Solution by homogeneous Precipitation Reaction (TiOCl2 수용액의 균일침전반응에 의한 나노크기의 브루카이트상 TiO2 분말제조)

  • Lee, Jeong-Hoon;Yang, Yeong-Seok
    • Korean Journal of Materials Research
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    • v.12 no.12
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    • pp.947-954
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    • 2002
  • HCl concentration and reaction time are the decisive factors in determining the structure of precipitates in the process of synthesis of $TiO_2$ particles from aqueous $TiOCl_2$ solution by precipitation and the volumetric proportion of brookite phase in $TiO_2$ particles can be controlled by these two factors. As reaction rate increases with increase of reaction temperature, the reaction time, at which maximum volumetric proportion of brookite phase in $TiO_2$ particles was obtained, was reduced. The brookite was transformed directly to rutile phase with only increase of reaction time. And precipitation was delayed with increase of HCl concentration because the amount of $H_2$O, which is necessary source of oxygen for conversion of $Ti^{+4}$ to $TiO_2$, was relatively reduced with increase of that. Brookite in the mixture phase powder was finally transformed to rutile phase via anatase through heat-treatment.

Synthesis of an Aspartame Precursor Using Thermolysin in Organic Two-Phase System (유기용매 이상계에서 Thermolysin에 의한 아스파탐 전구체 생산)

  • 이인영;안경섭;이선복
    • Microbiology and Biotechnology Letters
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    • v.20 no.1
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    • pp.61-67
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    • 1992
  • The synthesis of N-benzyloxycarbonyl-L-aspartyl-L-phenylalanine methyl ester(ZAPM), a precursor of aspartame, from N-benzyloxycarbonyl-L-aspartic acid(Z-Asp) and L-phenylalanine methyl ester hydrochloride(L-PM-HCl) was investigated in ethylacetate-MES buffer two-phase system using thermolysin. In organic two-phase system, the degree of spontaneous hydrolysis of L-PM. HCl was significantly reduced with increasing the volume ratio of organic to aqueous phase. Stability of thermolysin in organic two-phase system was found to be higher than that in MES buffer solution. More than 90% of initial enzyme activity was maintained after 10 days of incubation in case that the volume of organic phase was equal to that of buffer phase, while the half life of thermolysin was about 2 days in aqueous buffer solution. The results of partitioning of substrates and product in organic two-phase system showed that the difference in partition coefficients between substrates and product was maximum at pH 5.5. The optimal pH for 2-APM synthesis in organic two-phase system was found to be 5.5-5.8, which is consistent with the value expected from the partition experiments. As the concentration of substrates was increased the conversion yield of Z-APM was increased with concomitant reduction of L-PMqHC1 hydrolysis. In case that the concentration of L-PM-HCl and Z-Asp were 160 mM and 80 mM respectively, the conversion yield of Z-APM reached 90% after 28 hrs of reaction. The yield obtained at different volume ratio of organic phase compares well with the predicted equilibrium constant in biphasic system.

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Determination of Thiamine in Pharmaceutical Preparations by Reverse Phase Liquid Chromatography Without Use of Organic Solvent

  • Suh, Joon Hyuk;Kim, Junghyun;Jung, Juhee;Kim, Kyunghyun;Lee, Seul Gi;Cho, Hyun-Deok;Jung, Yura;Han, Sang Beom
    • Bulletin of the Korean Chemical Society
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    • v.34 no.6
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    • pp.1745-1750
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    • 2013
  • A novel green aqueous mobile phase modified with room temperature ionic liquids (RTILs) was employed in the absence of volatile organic solvents or ion-pairing reagents to analyze thiamine, a very polar compound, by reverse phase high performance liquid chromatography (RP-HPLC). Due to its strongly hydrophilic nature, thiamine was eluted near the column dead time ($t_0$) using a mobile phase without adding RTILs or ion-pairing reagents, even if a 100% aqueous mobile phase, which has weak elution power under reverse phase conditions, was used. Thus, 1-ethyl-3-methyl-imidazolium hexafluorophosphate ([EMIM][$PF_6$]), which has the strongest chaotropic effect, was selected as a mobile phase additive to improve retention and avoid baseline disturbances at $t_0$. Various mobile phase parameters such as cation moiety, chaotropic anion moiety, pH and concentration of RTILs were optimized to determine thiamine at the proper retention time. Method validation was performed to assess linearity, intra- and inter-day accuracy and precision, recovery and repeatability; all results were found to be satisfactory. The developed method was also compared to the current official United States Pharmacopoeia (USP) and Korean Pharmacopoeia (KP) methods using an organic mobile phase containing an ionpairing reagent by means of evaluating various chromatographic parameters such as the capacity factor, theoretical plate number, peak asymmetry and tailing factor. The results indicated that the proposed method exhibited better efficiency of thiamine analysis than the official methods, and it was successfully applied to quantify thiamine in pharmaceutical preparations.

반응추출을 이용한 당 지방산 에스테르의 분리정제

  • Seo, Deok-Gi;Kim, Gwang-Il;Kim, U-Gyeong;Yu, In-Sang;Yun, Hyeon-Hui
    • 한국생물공학회:학술대회논문집
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    • 2002.04a
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    • pp.504-507
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    • 2002
  • A separation/purification process for enzymatic sugar ester production was investigated The crude reaction mixture contained sugar ester and unreacted fatty acid in acetone. The reaction mixture was mixed with KOH/phosphate buffer. Hexane was then added to enhance phase separation. Three phases formed: a lower aqueous phase containing nothing of interest, a polar organic solvent middle phase that contained mostly fatty acid soaps, and a hexane-rich upper phase that contained mostly sugar ester. Distribution coefficient of each component was measured.

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Degradation of Trichloroethylene in Aqueous Phase by Electrochemical Ferrate(VI) (전기화학적 합성 Ferrate(VI)를 이용한 수중 Trichloroethylene 분해특성 연구)

  • Nam, Ju-Hee;Kwon, Byung-Hyuk;Kim, Il-Kyu
    • Journal of Korean Society of Water and Wastewater
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    • v.26 no.3
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    • pp.453-461
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    • 2012
  • The degradation characteristics of TCE by Ferrate(VI) oxidation have been studied. Ferrate(VI) were prepared by electrochemical method. The degradation efficiency of TCE in aqueous solution was investigated at various pH values, Ferrate(VI) doses and aqueous solution temperature values. GC-ECD was used to analyze TCE. TCE was degraded rapidly by ferrate(VI) in aqueous solution, Also, the experimental results showed that TCE removal efficiency increased with the increase of Ferrate(VI) doses. The effect of pH was investigated and the maximum degradation efficiency was obtained at pH 7. And intermediate products were identified by GC-MS techniques. Ethyl Chloride, Dichloroethylene, Chloroform, 1,1-dichloropropene, Trichloroacetic acid and Trichloroethane were identified as a reaction intermediate, and $Cl^-$ was identified as an end product.

Aqueous synthesis of quantum dots using functionalized ionic liquid (이온성 액체를 이용한 수계 양자 점 합성)

  • Choi, Suk-Young;Kim, Tae-Young;Suh, Kwang-S.
    • Proceedings of the Korean Institute of Electrical and Electronic Material Engineers Conference
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    • 2010.06a
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    • pp.254-254
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    • 2010
  • We report aqueous synthesis of cadmium telluride (CdTe) quantum dots(QDs) using imidazolium-based ionic liquids with various functional groups. The functinalized ionic liquids were designed to have thiol groups, and then phase transfer with aqueous or organic solvents can be adjusted by changing side chain lengths of the cation and the choice of anion. The quantum yield was obtained IL-functionalized CdTe QDs reached up to 40% by post-treatment method.

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Radical Intermediate Generation and Cell Cycle Arrest by an Aqueous Extract of Thunbergia Laurifolia Linn. in Human Breast Cancer Cells

  • Jetawattana, Suwimol;Boonsirichai, Kanokporn;Charoen, Savapong;Martin, Sean M
    • Asian Pacific Journal of Cancer Prevention
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    • v.16 no.10
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    • pp.4357-4361
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    • 2015
  • Thunbergia Laurifolia Linn. (TL) is one of the most familiar plants in Thai traditional medicine that is used to treat various conditions, including cancer. However, the antitumor activity of TL or its constituents has never been reported at the molecular level to support the folklore claim. The present study was designed to investigate the antitumor effect of an aqueous extract of TL in human breast cancer cells and the possible mechanism(s) of action. An aqueous crude extract was prepared from dried leaves of TL. Folin-Ciocalteu colorimetric assays were used to determine the total phenolic content. Antiproliferative and cell cycle effects were evaluated in human breast adenocarcinoma MCF-7 cells by MTT reduction assay, cell growth inhibition, clonogenic cell survival, and flow cytometric analysis. Free radical generation by the extracts was detected using electron paramagnetic resonance spectroscopy. The exposure of human breast adenocarcinoma MCF-7 cells to a TL aqueous extract resulted in decreases in cell growth, clonogenic cell survival, and cell viability in a concentration-dependent manner with an $IC_{50}$ value of $843{\mu}g/ml$. Treatments with extract for 24h at $250{\mu}g/ml$ or higher induced cell cycle arrest as indicated by a significant increase of cell population in the G1 phase and a significant decrease in the S phase of the cell cycle. The capability of the aqueous extract to generate radical intermediates was observed at both high pH and near-neutral pH conditions. The findings suggest the antitumor bioactivities of TL against selected breast cancer cells may be due to induction of a G1 cell cycle arrest. Cytotoxicity and cell cycle perturbation that are associated with a high concentration of the extract could be in part explained by the total phenolic contents in the extract and the capacity to generate radical intermediates to modulate cellular proliferative signals.

Toxicity Estimation of Nonionic Surfactants and Their Effect on the Biodegradation of Polycyclic Aromatic Hydrocarbons (PAHs) (비이온계 계면활성제의 독성 평가 및 Polycyclic Aromatic Hydrocarbons(PAHs) 생분해에 미치는 영향)

  • Park, Jong-Sup;Kim, In S.;Choi, Heechul
    • Journal of Korean Society of Environmental Engineers
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    • v.22 no.12
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    • pp.2107-2113
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    • 2000
  • Toxicity estimation of three nonionic surfactants (Brij 30, Tween 80, Triton X-lOO) and their effect on the biodegradation of polycyclic aromatic hydrocarbons (PAHs) in the aqueous phase and soil slurry phase were investigated. Brij 30 was found to be the most biodegradable among the surfactants tested, and showed no substrate inhibition up to a concentration of 1.5 g/L. It was definitely utilized as a carbon source by the microorganisms. Naphthalene and phenanthrene in the aqueous phase were completely degraded by phenanthrene-acclimated cultures within 60 hours, but a substantial amount of naphthalene was lost due to the volatilization. The limiting step in the soil slurry bioremediation was bioavailablity by the microorganisms in the sand slurry and mass transfer from a solid to aqueous phase in the clay slurry. TOC analysis revealed that most of substrates including surfactant in the reactor were degraded. pH transition indicated that phenanthrene was metabolized into intermediates containing acid function.

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