• Title/Summary/Keyword: Phase Separations

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Addition and Measurement of Modifier(Water) in Carbon Dioxide Mobile Phase for Supercritical Fluid Chromatography (초임계 유체 크로마토그래피에서 이동상에 Modifier를 첨가시키는 새로운 방법과 첨가된 Modifier(H2O) 양의 측정방법)

  • Ju Doweon;Pyo Dongjin
    • Journal of the Korean Chemical Society
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    • v.37 no.6
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    • pp.604-611
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    • 1993
  • Supercritical Fluid Chromatography(SFC) has become a technique for solving problems that are difficult by other chromatographic methods. However, the most widely used fluid, is no more polar than hexane. Polar samples which are difficult to be analyzed with pure supercritical C$O_2$ because of their high polarity can be separated by adding polar modifiers to supercritical C$O_2$. In this paper, a new method for monitering the mobile phase composition in modified supercritical fluid chromatography was developed. The amount of water dissolved in supercritical C$O_2$ was measured by amperometric microsensor which is made of thin film of perfluorosulfonate ionomer (PFSI). The amount of water dissolved in supercritical C$O_2$ stayed constant for a much longer time than with a saturator column. With this new mixing device, we could do good separations for insecticides and fungicides which are difficult to separate with pure C$O_2$.

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Comparison of QuEChERS and Solid Phase Extraction for Accurate Determination of Pesticide Residues in Kimchi Cabbage and Strawberry using Isotope Dilution Mass Spectrometry

  • Seonghee Ahn;Kebede Gebeyehu Mekete;Byungjoo Kim
    • Mass Spectrometry Letters
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    • v.14 no.4
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    • pp.178-185
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    • 2023
  • QuEChERS is used worldwide as a universal sample preparation method with many benefits, such as being quick, easy, cheap, effective, rugged and safe. This study examined whether QuEChERS can be employed in isotope dilution mass spectrometry (ID-MS) for accurate analysis of pesticides in food. The ratios of fortified values and measured values of malathion and fenitrothion using the QuEChERS method were compared with those using the solid phase extract (SPE) method which was previously used in this laboratory. The separations of the two pesticides on DB-5MS and VF-1701MS columns were compared. Malathion and fenitrothion were fortified into kimchi cabbage and pretreated with the QuEChERS method and the SPE method. The results obtained using the DB-5MS column varied according to the sample preparation method, column and pesticide level. Using the VF-1701 column, ratios were 98-102% by both QuEChERS and Carb/NH2 SPE method for all fortification level. Malathion and fenitrothion were fortified into strawberry samples for comparison with kimchi cabbage. The results for the strawberry samples indicated that the ratios were not influenced by the sample preparation methods or GC column. The QuEChERS method could be acceptable in the ID-MS method for pesticide residue analysis in food, however other conditions should be carefully considered for accurate determination, such as the column, amount of analyte and food matrix.

Purification and characterization of antifungal compounds produced by Bacillus subtilis KS1 (Bacillus subtilis KS1이 생산하는 항진균물질의 정제 및 특성)

  • Ryoo, Sung-Woo;Maeng, Hack-Young;Maeng, Pil-Jae
    • The Korean Journal of Mycology
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    • v.24 no.4 s.79
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    • pp.293-304
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    • 1996
  • A bacterial strain, KSl, possessing strong antifungal activity was isolated from soil samples of ginseng fields and identified as Bacillus subtilis. In greenhouse test, the culture filtrate of B. subtilis KS1 showed strong protective effect against several fungal diseases of agricultural plants such as cucumber gray mold and wheat leaf rust. In addition, the crude butanol fraction of the culture filtrate exhibited antagonistic effect against several fungi including plant or human pathogens, such as Botrytis maydis, Chytridium lagenarium and Candida albicans. The antifungal compound, SW1, produced by B. subtilis KS1 was purified through consecutive chromatographic separations on a pep-RPC column and a ${\mu}$ Bondapak $C_{18}$ reverse phase column. Temperature and pH showed little effect on the stability of the compound in the ranges $-20-121^{\circ}C$ and pH 4.0-10.0, respectively. The composition and structural characteristics of SW1 were analysed by HPLC and by $^1H-,\;^1H-^1H-COSY$, NOESY, COSY-NOESY and HOHAHA NMR spectroscopy, respectively, which revealed that the compound belongs to iturin A, a typical cyclic antifungal compound produced by B. subtilis. In contrast to the previously reported iturin A compounds which have one or no $-CH_3$ side chain in the hydrophobic hydrocarbon chain of ${\beta}-amino$ acids, SW1 was shown to have a ${\beta}-amino$ acid containing 12-carbon skeleton with two $-CH_3$ side chains.

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Scalable Fabrications of Mixed-Matrix Membranes via Polymer Modification-Enabled In Situ Metal-Organic Framework Formation for Gas Separation: A Review (고분자 변형으로 가능해진 MOF의 원위치 형성을 이용한 혼합기질 기체분리막의 대면적화 가능한 제막)

  • Sunghwan Park;Young-Sei Lee
    • Applied Chemistry for Engineering
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    • v.34 no.3
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    • pp.213-220
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    • 2023
  • Mixed-matrix membranes (MMMs), which are composed of a polymer matrix filled with high-performance fillers as a dispersed phase, have been intensively studied for gas separations for the past 30 years. It has been demonstrated that MMMs exhibit superior gas separation performance compared to polymer membranes and are more scalable than polycrystalline membranes. Despite their potential, the commercialization of MMMs has yet to be reported due to several challenging issues. One of the major challenges of MMMs is the non-ideal interface between the continuous polymer phase and dispersed phase, which can result in defect formation (i.e., interfacial voids, etc.). With respect, many MMM studies have focused on addressing the issues through scientific approaches. The engineering approaches for facile and effective large-scale fabrication of MMMs, however, have been relatively underestimated. In this review paper, a novel strategy for fabricating MMMs in a facile and scalable manner using in situ metal-organic framework (MOF) formation is introduced. This new MMM fabrication methodology can effectively address the issues facing current MMMs, likely facilitating the commercialization of MMMs.

Flow and Mechanical Properties of Linear and Branched Polycarbonates Blends (선형 및 분지화된 폴리카보네이트 블렌드의 기계적 성질과 유동특성)

  • 류민영;이재식;배유리
    • Polymer(Korea)
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    • v.24 no.1
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    • pp.38-47
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    • 2000
  • A study of linear and branched polycarbonates blend system is presented. Flow and mechanical properties, and miscibility were studied for the blends of various compositions. No phase separations were observed in the blend systems. The mechanical properties of blends were examined through tensile strength, tensile modulus, flexural strength, flexural modulus and impact strength. Melt viscosity, storage and loss moduli of the blends with various compositions were examined at various temperatures. The dependence of viscosity on molecular weight was also presented. Flow properties of the blends showed significant variations however, mechanical properties were relatively independent of the compositions. As the content of branched polycarbonate increased, the dependence of viscosity on molecular weight and shear thinning behavior became more marked. Therefore the blend systems which have same mechanical properties but different flow properties can be obtained.

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Quantitative Analysis of the Marker Constituents in Yongdamsagan-Tang using Liquid Chromatography-Electrospray Ionization-Tandem Mass Spectrometry (LC-ESI-MS/MS를 이용한 용담사간탕의 주요 성분 분석)

  • Seo, Chang-Seob;Ha, Hyekyung
    • Korean Journal of Pharmacognosy
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    • v.48 no.4
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    • pp.320-328
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    • 2017
  • Yongdamsagan-tang has been used to treat the urinary disorders, acute- and chronic-urethritis, and cystitis in Korea. In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous analysis of the 20 bioactive marker compounds, geniposidic acid, chlorogenic acid, geniposide, liquiritin apioside, acteoside, calceolarioside B, liquiritin, nodakenin, baicalin, liquiritigenin, wogonoside, baicalein, glycyrrhizin, wogonin, glycyrrhizin, wogonin, saikosaponin A, decursin, decursinol angelate, alisol B, alisol B acetate, and pachymic acid in traditional herbal formula, Yongdamsagan-tang. Chromatographic separations of all marker compounds were conducted using a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was performed using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization source in the positive and negative modes. The flow rate was 0.3 mL/min and injection volume was $2.0{\mu}L$. The correlation coefficient of 20 marker compounds in the test ranges was 0.9943-1.0000. The limits of detection and quantification values of the all marker components were 0.11-6.66 and 0.34-19.99 ng/mL, respectively. As a result of the analysis using the optimized LC-ESI-MS/MS method, three compounds, geniposidic acid (from Plantaginis Semen), alisol B (from Alismatis Rhizoma), and pachymic acid (from Poria Sclerotium), were not detected in this sample. While the amounts of the 17 compounds except for the geniposidic acid, alisol B, and pachymic acid were $0.04-548.13{\mu}g/g$ in Yongdamsagan-tang sample. Among these compounds, baicalin, bioactive marker compound of Scutellariae Radix, was detected at the highest amount as a $548.13{\mu}g/g$.

A Minerlogical Study of Plagioclase in Volcanic Rocks from the Mt. Mudeung Area (무등산지역 화산암류에서 산출되는 사장석의 광물학적 연구)

  • Park Byung-Kyu;Kim Yong-Jun;Kim Youn-Joong
    • Journal of the Mineralogical Society of Korea
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    • v.18 no.3 s.45
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    • pp.155-164
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    • 2005
  • Volcanic rocks from the Mt. Mudeung area which are composed of Hwasun andesite, Mudeungsan dacite and Togok rhyolite contain plagioclase phenocrysts in common. Majority of the repeated twins observed in optical microscopy are albite twin and some are pericline twin. EPMA studies of plagioclases from Hwansun andesite, Mudeungsan dacite and Togok rhyolte indicate calcic andesine, andesine-oligoclase, nearly pure albite, respectively Albite twin and pericline twin can be easily distinguished through TEM diffraction patterns, which is quite difficult by optical microscopy. Plagioclases in volcanic rocks from the Mt. Mudeung area do not show e-reflection in (100) electron diffraction patterns, probably because of their high cooling rate, which inhibited phase separations during cooling.

Development of Chemical Separation Process for Thallium-201 Radioisotope with Lead Standard Material (납 표준물질을 이용한 방사성동위원소 Thallium-201의 화학적 분리공정 개발)

  • JunYoung Lee;TaeHyun Kim;JeongHoon Park
    • Journal of Radiation Industry
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    • v.17 no.4
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    • pp.543-549
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    • 2023
  • Thallium-201 (201Tl) is a medical radioisotope which emits gamma rays when it decays and used in myocardial perfusion scans in single-photon emission tomography due to its similar properties to potassium. Currently, the Korea Institute of Radiological & Medical Sciences is the only institution producing 201Tl in Korea, and optimization of 201Tl production research is necessary to meet supply compared to domestic demand. To this end, technical analysis of plating target production and chemical separation methods essential for 201Tl production research is conducted. It deals with the process of generating and separating 201Tl radioisotope and target production, It can be generated through a nuclear reaction such as natHg(p,xn)201Tl, 201Hg(p,n)201Tl, natPb(p,xn)201Bi → 201Pb → 201Tl, 205Tl(p,5n)201Pb → 201Tl, and considering impure nuclide generated simultaneously with the use of proton beam energy of 35 MeV or less, it is intended to be produced using the 203Tl(p,3n)201Pb→201Tl nuclear reaction. In particular, the chemical separation of Tl is a very important element, and the chemical separation methods that can separate it is broadly divided into four types, including solid phase extraction, liquid-liquid, electrochemical, and ion exchange membrane separation. Some chemical separations require additional separation steps, such as methods using selective adsorption. Therefore, this technical report describes four chemical separation methods and seeks to separate high-purity 201Tl using a method without additional separation steps

Isolation and Identification of Antimicrobial Compounds against Helicobacter pylori from Rosemary (Rosmarinus officinalis L.) Extracts (로즈마리(Rosmarinus officinalis L.) 추출물로부터 Helicobacter pylori에 대한 항균물질 분리 및 동정)

  • Yoon, So-Jung;Kim, Jin-Sung;Jo, Bun-Sung;Kim, Jeung-Hoan;Lee, Sun-Ho;Ahn, Bong-Jeun;Cho, Young-Je
    • Journal of Applied Biological Chemistry
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    • v.54 no.3
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    • pp.159-165
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    • 2011
  • Rosmarinus officinalis extracts had a significant antimicrobial activity against Helicobacter pyori. Total phenolic contents and inhibition zone of rosemary extracts were estimated to be 25.7 mg/g and 14 mm at $200{\mu}g/mL$ of phenolic contents, respectively. The Sephadex LH-20 and MCI-gel CHP-20 column chromatographic separations for the phenolic extracts from R. officinalis leaves led to isolation of five acids, whose structures were determined as protocatechuic acid (A), coumaric acid (B), caffeic acid (C), chlorogenic acid (D), and rosmarinic acid (E), from interpretation of spectroscopic data including nagative fast atom bombardment (FAB)-mass, $^1H$-NMR, $^{13}C$-NMR, and IR. All isolated compounds were tested for antimicrobial activity against H. pyori. The purified single compound showed less antimicrobial activity against H. pylori than the mixed purified compounds, which generate A+B, A+E, C+D, C+E (each $200{\mu}g/disc$) excellent as large clear zone by synergy effect. These results indicate rosemary extracts are preventive agents against H. pyori.

High Permeability, High Selectivity Carbon-Silica Membranes for Gas Separation (기체분리용 고투과선택성 탄소-실리카막)

  • 이영무;박호범
    • Membrane Journal
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    • v.12 no.2
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    • pp.107-119
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    • 2002
  • Carbon-silica ($C-SiO_2$) membranes can be easily prepared by the pyrolysis of two-phase copolymers containing an aromatic imide block and a siloxane block and remarkably high permselectivities of $He/N_2, O_2/N_2,$ and $CO_2/N_2$. The pyrolysis of the imide-siloxane block copolymers was carried out at different final temperatures, $600^{\circ}C, 800^{\circ}C,$ and $1000^{\circ}C$ under an inert atmosphere, and is the first reported case of the precursors being used for the preparation of carbon membrane. The polymeric precursors were synthesized in a wide range of siloxane content and different final morphology, and the pyrolozed membranes were tested with a high vacuum time-lag method at $25^{\circ}C$ and 76cmHg of feed pressure. In experiments with He, $CO_2, O_2 \;and \;N_2$, the membranes were found to have good $O_2/N_2$ selectivity up to 32.2 and $O_2$ permeability on the order of $10-8/cm^2(STP)cm/cm^2seccmHg.$.