• Title/Summary/Keyword: methanol separation column

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Separation of Caffeine and Catechin Compounds from Green Tea by Quercetin Molecular Imprinted Solid-Phase Extraction (케르세틴 분자각인 고정상 추출을 이용한 녹차에서 카페인 및 카테킨 화합물의 분리)

  • Jin, Yin-Zhe;Row, Kyung-Ho
    • Journal of the Korean Chemical Society
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    • v.51 no.2
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    • pp.165-170
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    • 2007
  • In this work, caffeine and some catechin compounds such as +C, EGC and EGCG were extracted from green tea using quercetin molecular imprinted polymers in solid-phase extraction. For synthesis of MIP, quercetin as the templates, MAA as the monomer, EGDMA as the crosslinker and AIBN as the initiator were used. For extraction of caffeine and catechin compounds from green tea, the solid-phase extractions of a load followed by wash and elution procedures were done with water, methanol and methanol:acetic acid=90:10 (vol.%) as the solvents, respectively. HPLC analysis (C18 column, 5 μm, 250×4.6 mm) with the mobile phase of methanol:water=40:60 (vol.%) at a flow rate of 0.5 ml/min was adopted for the quantitative determination. By solid-phase extraction, the resolutions of caffeine and some catechin compounds from green tea were increased. The quercetin-MIP had higher selectivity to +C compounds.

Antifungal Mechanism and Properties of Antibiotic Substances produced by Bacillus subtilis YB-70 as a Biological Control Agent

  • Kim, Yong-Su;Kim, Sang-Dal
    • Journal of Microbiology and Biotechnology
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    • v.4 no.4
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    • pp.296-304
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    • 1994
  • Antibiotic substances were produced by Bacillus subtilis YB-70, a potential biocontrol agent found to suppress root-rot of eggplant (Solanum melonggena L) caused by Fusarium solani, in a dextrose glutamate medium and isolated by isoelectric precipitation. Partial purification was performed by column chromatography on silica gel with two solvent systems: chloroform-methanol and methanol-chloroform-water as eluting solvents, This active fraction YBS-1 s contained antifungal activity were soluble in ethanol, methanol, and water, but were not soluble in other solvents including acetone, butanol, ethyl ether, dimethylformamide, propanol, and etc. High performance liquid chromatography and thin layer chromatographic separation of YBS-1s showed that they have been composed of three biological active bands that were named YBS-1A, -1B, and -1C. The substances were stable to heat and resistant to protease. YBS-1s were active against a wide range of plant pathogenic fungi but did not inhibit the growth of bacteria and yeasts. They were not only fungicidal but also fungistatic against chlamydospores of F. solani. The $ED_{50}$ values for the chlamydospore germination and the germ-tube growth of F. solani were $O.725\mu\textrm{m}/ml\;and\;O.562\mu\textrm{m}/ml$, respectively. Microscopic observations proved the substances restricted the growth of phytopathogenic fungus F. solani by spore burst followed by dissolving of its germ-tube, and caused abnormal hyphal swelling after application to chlamydospores or growing hyphae. Cultural filtrate of B; subtilis YB-70 also suppressed the development of root-rot of eggplant in pot tests.

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Quantitatation of Benzoic and Sorbic Acids in Some Processed Foods of Korea (일부 한국 가공식품의 벤조산과 소르빈산의 함량 조사)

  • Mitra, Sanika;Han, Jang-Il;Lee, Ki-Teak;Kim, Seong-Ai
    • Food Science and Preservation
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    • v.16 no.6
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    • pp.789-796
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    • 2009
  • Benzoic acid (BA) and sorbic acid (SA) are the preservatives most commonly used in food. Although BA and SA are generally safe, some previous studies have shown that consumption of excessive amounts of these food additives can be a health hazard. The aim of this study was to determine the amounts of BA and SA in processed foods in Korea. Different brands of fruit juice, yogurt, cheese, dried fruits, jam, and margarine were purchased at a local market in Daejeon, Korea. Samples were analyzed by high-performance liquid chromatography (HPLC) using a UV detector. Chromatographic separation was achieved with a C18 column. Methanol acetate buffer (pH 4.4) at a 35:65 v/v ratio was used as the initial mobile phase to elute BA and SA. The detector wavelength was set at 254 nm. The average test results observed for BA concentrations in fruit juice, yogurt, cheese, dried fruits, jam, and margarine were $40.26{\pm}0.02$, $2.07{\pm}0.06$, $0.02{\pm}0.09$, $0.36{\pm}08$, $265.30{\pm}0.02$, and $27.34{\pm}0.08\;mg/kg$, respectively. Average concentrations of SA in these samples were $0.92{\pm}0.06$, $1.06{\pm}0.07$, $7.30{\pm}0.01$, $14.14{\pm}0.08$, $25.65{\pm}0.06$, and $4.81{\pm}0.07\;mg/kg$, respectively. Thus, the average levels of BA and SA in the studied food items were lower than the KFDA-permitted limits. Moreover, the estimated daily intake of both BA and SA by a typical consumer were below the maximum recommended daily values.

Dynamic Optimization of a Reactive Distillation Column Producing Methyl Acetate (메틸 아세테이트 생산을 위한 반응증류 공정의 동적 최적화)

  • Kim, Jiyong;Kim, Junghwan;Moon, Il
    • Korean Chemical Engineering Research
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    • v.46 no.4
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    • pp.739-746
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    • 2008
  • The aim of this study is finding the optimal design parameters and the optimal operation variables of a reactive distillation column. Different from steady state optimization, dynamic optimization makes it possible considering operation ability as well as design problems at process design step. For performing dynamic optimization, dynamic simulation should be done first. If dynamic simulation is already finished, dynamic optimization can be performed with less effort than that of dynamic simulation.Reactive distillation systems involving reaction and separation in a single unit have the potential to reduce capital and operating costs, particularly when reaction have conversion constraint or when azeotropes exist making conventional separation difficult and expensive. This study here present work on the continuous distillation process, the homogeneous catalyzed esterification of methanol and acetic acid, the synthesis of methyl acetate. Based on an equilibrium stage model of a reactive distillation column a dynamic optimization problem was formulated and solved. And the results were verified by performing dynamic simulation and showing the variation of conversion and purity as the variation of the operation variables. As the results of dynamic optimization, this study found optimal feed ratio, reflux ratio and reboiler duty of this system. And as this study applied it to dynamic simulations the dynamic characteristics of a reactive distillation column are showed under optimal operating condition.

Spectrophotometric Determination of Iron with 2-Hydroxybenzaldehyde-5-nitro-pyridylhydrazone after Separation with Amberlite XAD-7 Nonionic Resin (Amberlite XAD-7 비이온성 수지로 분리 후 2-Hydroxybenzaldehyde-5-nitro-pyridylhydrazone을 이용한 철의 분광학적 정량)

  • Park, Chan Il;Chung, Byung Doo;Jung, Duck Chae;Cha, Ki Won
    • Journal of the Korean Chemical Society
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    • v.43 no.5
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    • pp.522-526
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    • 1999
  • 2-Hydroxybenzaldehyde-5-nitro-pyridylhydrazone (2HB-5NPH) was synthesized and its application to the spectrophotometric determination of iron was studied. The reagent reacts with iron in the pH range 6.0-7.5 to form a yellow coIored 1:2 chelate which is very stable in methanol solution. Beer's law is obeyed in the concentration range 0.05∼2.0 ${\mu}gmL^{-1}$ iron and separation procedure using a short column filled with Amberlite XAD-7 nonionic chelating resin is proposed for the spectrophotometric determination of traces of iron. The influence of several ions as interference was discussed. The separation of Fe(III) ion from the mix-ture solution were carried out with the buffer solution (pH 5.0) and 0.25M HCl as eluents.

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Factors Affecting HETP in Preparative Liquid Chromatography (제조용 액체 크로마토그래피에서 HETP에 영향을 미치는 인자)

  • Choi, Du Chan;Choi, Dai-Ki;Row, Kyung Ho
    • Applied Chemistry for Engineering
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    • v.7 no.5
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    • pp.985-991
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    • 1996
  • In chromatographic separation, HETP(height equivalent to a theoretical plate) is a useful quanititive parameter and it is wildely designated as column efficiency. The effects of operating conditions (sample concentration, injection volume, flow rate and mobile phase composition) on HETP were investigated in perparative liquid chromatography (PLC). Water and organic modifier of methanol were used as mobile phase. The sample of thymidine was injected into preparative C18 columns. The system was run by a isocratic mode in 1.5~5.5ml/min. The larger amounts of sample and higher flow rates of mobile phase increased HETP, which means that column efficiencies were worse. As the weight of sample injected into a chromatographic system could be prepared with different concentrations and injection volumes, for the same amount of sample, HETP was approximately increased two times with the ten-fold injection volume. HETP was mainly affected by the resistance of stationary and mobile phase mass transfer in the intraparticle section of packings at higher velocities.

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Studies of separation and quantitation for selenium species in food (식품중의 셀레늄 화학종의 분리 및 정량연구)

  • Jang, Hee-Young;Min, Hyungsik;Lee, Jonghae;Pak, Yong-Nam
    • Analytical Science and Technology
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    • v.26 no.3
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    • pp.182-189
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    • 2013
  • The purpose of this research is to separate and quantitate selenium species in some food samples with HPLC-ICP-MS. Cation exchange chromatography showed efficient separation only for inorganic Se species while reversed phase ion pair chromatography showed good separation for both inorganic and organic Se species. $C_8$ column ($Symmetryshield^{TM}\;RP_8$, 3.5 ${\mu}m$, $4.6{\times}150$ mm) was used with optimum condition of 5% methanol mobile phase, 0.05% of nonafluorovaleric acid ion pairing reagent. Five standard Se species of Se(IV), Se(VI), SeCys(selenocystein), SeMet(selenomethionine) and Se-M-C(seleno methyl cystein) were separated successfully under the optimum condition (mobile phase; 5% methanol, ion-pairing reagent; 0.05% nonafluorovaleric acid, flow rate; 0.9 mL $min^{-1}$). To extract Se species, microwave assisted and enzyme-assisted extraction methods were studied. In enzyme-assisted extraction method, protease I for garlic, protease I plus trypsin for pork and mackerel, and protease XIV for tuna showed the best extraction efficiency. With the optimum condition for each sample, it was found that mostly inorganic Se, SeCys and SeMet are present in the sample studied ranging from few ${\mu}g$ $g^{-1}$ to few tens of ${\mu}g$ $g^{-1}$.

Effect of Solidago altissima L. Extract on Forage Crop Germination

  • Ho-Jun Gam;Yosep Kang;Eun-Jung Park;Ki-Yong Kim;Sang-Mo Kang;In-Jung Lee
    • Proceedings of the Korean Society of Crop Science Conference
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    • 2022.10a
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    • pp.114-114
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    • 2022
  • There are 28 families and 166 species of exotic weeds on agricultural land and among these, 23 families and 80 species of exotic weeds occur on pastures. Among them, the Solidago altissima is a perennial weed belonging to the asteraceae family and it is an exotic weed that spreads to the surrounding area using methods such as high seed production, vegetative propagation using underground rhizomes and allelochemical. Accordingly, in 2009, the Ministry of Environment designated it as an ecosystem-disrupting species. This study was conducted to obtain basic data about the effects of S.altissima derived allelochemicals on forage crops. The root of S.altissima was separated, dried in the shade and then pulverized to prepare an root powder. Powder was repeatedly extracted with methanol for 3 days and concentrated under reduced pressure to obtain an root methanol extract. Dissolve the extract in distilled water, dispense it in a separate-funnel and proceed with liquid-liquid extraction by adding equal amounts of n-haxane (Hex), chloroform (CHCI3), ethyl acetate (EtoAC), and butanol (BuOH) in order of increasing polarity. A seed-bioassay was performed using fractions for each solvent, followed by separation and purification by silica gel column chromatography. As a result of the fraction germination test for each solvent, the IC50 values using the fresh weight of each fraction were 898.3 mg L-1, 676.3 mg L-1, 1160 mg L-1 and 1360 mg L-1. CA, CB, and CC fractions were obtained through primary silica gel column chromatography that used CHCI3 fraction. As a result of seed-bioassay using each fraction, the IC50 values for the fresh weight of each fraction was 537.3 mg L-1, 1280 mg L-1 and 1947 mg L-1. Based on this, 5 fractions were obtained as a result of secondary silica gel column chromatography using the CA fraction. A seed-bioassay was performed, as a result, the lowest IC50 value was calculated as 226.7 mg L-1 in the CAE fraction. Based on this, the fraction was analyzed by GC-MS. The results of this study can be used as basic research data on the effects of weeds on forage crops and allelochemicals secreted from S. altissima.

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A Study on the Analysis of Isothiazolinone Components by High Performance Liquid Chromatography (고성능액체크로마토그래피에 의한 Isothiazolinone Components의 분석에 관한 연구)

  • 김종규;이덕희
    • Journal of Environmental Health Sciences
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    • v.18 no.2
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    • pp.102-105
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    • 1992
  • Introduction : Isothiazolinone product is one of new preservatives used in cooling tower, paper mill, and general industrial waters.l) It is also effective in controlling bacteria and fungi in the manufacture and storage of dispersed pigments, such as kaolin clays, titanium dioxide, calcium carbonate and others\ulcorner Its broad-spectrum activity, excellent physical and chemical compatibility with anionic, nonionic and cationic surfactants and most organic and inorganic compounds and low toxicity at recommended use levels provide formulators with an effective, economical, and environmentally acceptable alternative to other commercial biocides. It dose not contain or generate formaldehyde and is easy to formulate (1.5% solution is supplied as an aqueous solution), so that it gains advantage over the other preservatives. The active ingredients of the isothiazolinone product are unchlorinated compound (2-methyl-4-isothiazolin-3-one) and chlorinated one (5-chloro-2-methyl-4-isothiazolin-3-one). Methods preferred for the analysis of preservatives are chromatographic methods, especially high performance liquid chromatograph (HPLC). Although several methods were satisfactory in respect to separation, no offical method has been published for the isothiazolinone components. This study was performed to search for an alternative method in order to show flexible operating conditions of HPLC and to reduce assay time.

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Separation and Performance lest of Wnitening Agent in Rhodiola Sachalinensis (홍경천에 포함된 미백성분의 분리 및 성능검사)

  • 최두영;안소영;이승기;한정선;김은철;이향복;신정현;김은기;노경호
    • KSBB Journal
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    • v.19 no.3
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    • pp.169-173
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    • 2004
  • The Rhodiola Sachalinensis 5 g were mixed and extracted with methanol 150 $m\ell$ at the room temperature for 12 h. The effluents were collected and grouped into the two. Un this experimental condition, the mobile phase composition were linearly changed as follows; water/methanol : 90/10 - 30/70 (vol. %, for 5 min), 30/70 - 10/90 (vol. %, for 15 min) and an analytical column (3.9 ${\times}$ 25 em, 15 $\mu\textrm{m}$ particle size, and 300 ${\AA}$ pore size) was utilized. The performance of the extracted Rhodiola Sachalinensis as a whitening agent was not favorable, so it classifies the Rhodiola Sachalinensis extractions with two fractions and collects each fraction for whitening agent assay. For the in-vivo melanin production ratio assay that used melanin-a cell in 10 ppm concentration, it was 58.6%, the first fraction of the effluents collected between 1.0 and 4.0 min, while it was 60% between 10.4 and 17.6 min for the second fraction, which were more efficient than that of arbutin, 45.6%.