• Title/Summary/Keyword: 고정상 컬럼

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Optimizing analytical method in Health Functional Food code with adjustable chromatographic parameters: A case study of vitamin C (건강기능식품공전 시험법의 크로마토그래프법 조건의 조정 및 비타민C에 대한 적용성 평가 연구)

  • Junghoon Shin;Yooseong Jeong;Yong Seok Choi;Sang Beom Han;Dong-Kyu Lee
    • Analytical Science and Technology
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    • v.37 no.3
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    • pp.143-154
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    • 2024
  • In this study, we improved the vitamin C test method and reviewed data on the adjustable range of chromatography conditions for quantification. First, we adjusted the mobile phase conditions such as solvent composition, salt concentration, pH and column temperature and in particular, it was confirmed through an improved test method that the peak derived from the buffer solution could be clearly separated from the target component, vitamin C by adjusting the pH. The retention time of vitamin C was partially changed by adjusting the column diameter, length and particle size but the number of theoretical plates indicated similar values and did not affect the separation and quantitative analysis of the target component. The flow rate according to the column specifications was derived from the equation proposed by the U.S. FDA (Food and Drug administration) and the Korean MFDS (Ministry of Food and Drug Safety), and evaluation of the applicability to vitamin complexes showed high selectivity for vitamin C even with altered stationary phase conditions and flow rates. In conclusion, vitamin C can be optimally separated and detected by changing the chromatographic method conditions and it was confirmed that the mobile and stationary phase conditions of liquid chromatography can be slightly adjusted in case the assay method uses an isocratic elution.

Preparation of Microcolumns Made of Glass-Lined Stainless Steel Tubing or Other Materials and Their Chromatographic Application (내벽이 유리로 코팅된 스테인레스 스틸 관 및 기타 재질을 이용한 마이크로 컬럼의 제작과 그의 크로마토그래피 응용에 관한 연구 (Ⅱ))

  • An, Hyun Joo;Cheong, Won Jo
    • Journal of the Korean Chemical Society
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    • v.39 no.11
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    • pp.863-868
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    • 1995
  • We have prepared microcolumns made of stainless steel tubing, glass-lined stainless steel tubing, and silica-lined stainless steel tubing and examined their performances comparatively. The length of columns was fixed as 30 cm, and the I.D.'s, either 1 mm or 0.5 mm. Octadecyl bonded silica paticles $(5\mu)$ were used as the stationary phases. p-Nitroaniline, N,N-dimethyl-o-nitro-p-toluidine,and ethylbenzene were used as the test solutes. The glass-lined or silica-lined stainless steel columns showed better performances than the plain stainless steel column did. The number of theoretical plates over 10,000 were obtained even for the 0.5 mm I.D. (30 cm long) column as long as the glass-lined stainless steel tubing was used.

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Degradation of a Pesticide, 4-Chloro-2-methylphenoxyacetic Acid by Immobilized Biofilm in Bench-scale Column Reactors (컬럼반응조내에서의 고정된 생물막에 의한 농약 4-chloro-2-methylphenoxyacetic acid의 분해)

  • 오계헌;차민석
    • KSBB Journal
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    • v.11 no.5
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    • pp.524-528
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    • 1996
  • Bacterial degradation of 4-chloro-2-methylphenoxyacetic acid (MCPA) was studied in column reactors under conditions approximating a fluidized bed system, with granular activated carbon (GAC) as a support matrix. A mixed bacterial culture of MCPA-degrading bacteria was used as an inoculum to develop a biofilm on GAC. Initially, adsorption of MCPA by GAC and blofilm formation on GAC were examined. MCPA degradation was evaluated with a batch and continuous mode of operation of the GAC fixed-film column reactors. In the batch operations, complete degradation of MCPA was achieved during the incubation period. Partial degradation of MCPA occurred in the continuous operations and MCPA degradation was dependent on the feeding rate of MCPA solution.

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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.

Simultaneous detection of residual fungicide in Bean Sprouts by Solid-phase Extraction (고체상 추출법에 의한 콩나물 중의 잔류농약 동시 검출)

  • Lee, Myunghwoon;Lee, Taejoon;Pyo, Dongjin
    • Analytical Science and Technology
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    • v.6 no.5
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    • pp.509-514
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    • 1993
  • Benomyl, topsin-M and thiram been known as one of the seed disinfectant. For these studies benomyl, topsin-M and thiram simultaneously had been analyzed by high performance liquid chromatographic method using ODS cartridge, benomyl, topsin-M and thiram was chromatographed using an ODS column and eluent 40% Acetonitrile at a flow rate of 1ml/min. The UV Detector responses at 276nm.

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Isolation and Purification of Bioactive Materials Using High-Performance Counter-Current Chromatography (HPCCC) (고속역류크로마토그래피 기술을 이용한 생리활성 물질의 분리 및 정제)

  • Jung, Dong-Su;Shin, Hyun-Jae
    • KSBB Journal
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    • v.25 no.3
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    • pp.205-214
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    • 2010
  • Many successive liquid-liquid extractions occur enabling purification of the crude material to occur. In high performance counter-current chromatography (HPCCC), crude material is partitioned between two immiscible layers of solvent phases. The stationary phase (SP) is retained by hydrodynamic force field effect and the mobile phase (MP) is pumped through the column. Purification occurs because of the different solubility of the components in the liquid mobile and stationary phases. There are many key benefits of liquid stationary phases such as high mass and volume injection loadings, total sample recovery, and easy scale-up. Many researchers showed that predictable scale-up from simple test is feasible with knowledge of the stationary phase retention for the planned process scale run. In this review we review the recent advances in HPCCC research and also describe the key applications such as natural products and synthetics (small or large molecules).

Adsorption Characteristics of Pb(II) and Cr(III) onto C-Methylcalix[4]resorcinarene (C-Metylcalix[4]resorcinarene에서 Pb(II)와 Cr(III)의 흡착 특징)

  • Jumina, Jumina;Sarjono, Ratnaningsih Eko;Siswanta, Dwi;Santosa, Sri Juari;Ohto, Keisuke
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.454-462
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    • 2011
  • A study on the adsorption characteristics of Pb(II) and Cr(III) cations onto C-methylcalix[4]resorcinarene (CMCR) has been conducted. CMCR was produced by one step synthesis from resorcinol, acetaldehyde, and HCl. Most parameters in batch system confirm that CMCR is a good adsorbent for Pb(II) and Cr(III). Cr(III) uptake was bigger than that of Pb(II), but Cr(III) adsorption rate was slower than Pb(II). The adsorption kinetic of Pb(II) and Cr(III) adsorptions in batch followed pseudo $2^{nd}$ order kinetics model, but the kinetic of Pb(II) adsorption in fixed bed column system followed first order model. Desorption studies to recover the adsorbed Pb(II) was performed sequentially with distilled water and HCl, and the results showed that the adsorption was dominated by chemisorption.

Effects of pH and Potassium Chloride in Solvent System of High-Speed Countercurrent Chromatography (pH 및 염화칼륨 첨가가 고속역류크로마토그래피의 용매시스템에 미치는 영향)

  • Lee, Chang-Ho;Lee, Boo-Yong;Lee, Hyun-Yu;Lee, Cherl-Ho
    • Korean Journal of Food Science and Technology
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    • v.29 no.6
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    • pp.1222-1227
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    • 1997
  • Effects of the physical properties of solvent system such as pH and polarity change by salt addition in solvent system were investigated by using high speed countercurrent chromatography apparatus (Model CCC-1000, Pharm-Tech Research Corp. USA). The changes of pH and interfacial tension in solvent system of high speed countercurrent chromatography did not significantly affect on retention of stationary phase, but induced remarkable changes in the partition coefficient of ginkgo flavonoids, kaempferol, quercetin and isorhamnetin. The partition coefficients of ginkgo flavonoid standard increase with an increased pH of solvent system and quercetin sharply increased at pH 10.0. Retention of stationary phase decreases with an increased concentration of KCl in butanol of solvent system. Interfacial tension between two phase in solvent system of hexane increases with an increased concentration of KCl. The polarity of solvent system significantly changes the partition coefficients of ginkgo flavonoid.

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Phenol Concentration using Thermal Simulated Moving Bed Concentrator (TSMBC(Thermal Simulated Moving Bed Concentrator)를 이용한 페놀 농축)

  • Gil, Mun-Seok;Kim, Jin-Il;Lee, Ju Weon;Koo, Yoon-Mo
    • Korean Chemical Engineering Research
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    • v.50 no.6
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    • pp.1027-1033
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    • 2012
  • Conventional SMB process is operated using 4-zone having several chromatography columns in each zone. Unlike batch chromatography, SMB process can continuously separate binary materials. Both high productivity and purity are obtainable by using SMB process. In this study, the simulation on Thermal Simulated Moving Bed Concentrator (TSMBC) which is a SMB process with thermal swing adsorption was carried out. The advantage of TSMBC is that adsorption isotherm can be easily controlled by thermal wave or direct heating. Recovery of pure water and concentration of phenol was studied in simulation. To verify environmental-friendly potential of TSMBC, DOWEX $1{\times}4$ was chosen as an adsorbent and phenol was selected as a target material. When 3 columns were used in this study, concentration of phenol is 2.29, 2.28 and 1.31 times higher than injected sample. However, a contamination of phenol in solvent port was found, probably due to the restriction of adsorption isotherm of phenol on DOWEX $1{\times}4$.

기체 크로마토그래피법을 이용한 수소동위원소 분리기술

  • 김광락;구제휴;나정원;정흥석;성기웅;김용익
    • Nuclear Engineering and Technology
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    • v.28 no.1
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    • pp.93-101
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    • 1996
  • 수소동위원소의 실험과 취급 및 삼중수소 제거시설의 운용이나 더 나아가서 핵융합소재의 관리기술을 위해서는 수소동위원소분만 아니라 그들의 이성질체들에 대한 정성 및 정량분석이 필수적이며 이를 위해 기체크로마토그래피 분리법이 중요한 분석수단으로 활용되어오고 있다. 본 연구에서는 고순도 $H_2및$ $D_2의$ 수소동위원소 기체를 대상으로 하고 상용의 기체크로마토그래피 분석기를 사용하여 분리컬럼 분위기를 액체질소온도로 유지하고 헬륨 케리어기체를 특별제작된 진공-시료주입장치를 통해 펄스주입하여 크로마토그래피 분리실험을 수행하였다. 10%함량의 염화망간으로 부분 비활성화 시킨 산화알루미늄을 고정상으로 선정하여 이성질체의 분리를 억제할 수 있었으며 흡착후 분리용리시간이 단축된 비교적 좋은 수소동위원소 분리조건을 실증하므로서, 저농도 수소동위원소의 정량분석과 고순도 수소동위원소의 분리 및 농축기술 개발을 위한 기초를 마련하였다.

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