• Title/Summary/Keyword: eluent

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Isolation and Characterization of Major Glycosphingolipid from Rice Bran Extract (쌀겨 추출물로부터 스핑고당지질의 분리와 구조결정)

  • Mitsutake, Susumu;Okada, Tadashi;Kang, Byoung-Won
    • Applied Biological Chemistry
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    • v.50 no.1
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    • pp.72-76
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    • 2007
  • In order to examine the biofunctions of glycosylceramide which is representative of sphingolipid, monoglycosylceramide (cerebroside) was isolated from rice bran extract. Crude glycosylceramides were isolated in large quantities and promptly by flash system column chromatography from rice bran extract, and purified by normal-phase HPLC using an evaporative light-scattering detector. One major cerebroside was obtained by HPLC used as an eluent consisting of chloroform, methanol and water (99:11:1, v/v/v), and the constituents were analyzed by MALDI/TOF-MS, FAB-MS, GC and 600 MHz $^1$H-NMR. The component sugar was estimated to be glucose. In the ceramide, the fatty acid component consist was 2-hydroxy arachidic acid. The long-chain base component was sphinga-4,8-dienine.

Structural Analysis of Natural Indigo Colorants Extracted from polygonum tintorium (쪽풀에서 추출한 천연 인디고 색소의 구조 분석)

  • 정인모;김인회;남성우
    • Textile Coloration and Finishing
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    • v.10 no.3
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    • pp.20-28
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    • 1998
  • Natural indigo colorants were prepared by extraction of polygonum tintorium which was harvested just in the blooming season(in the late of July). The components were analyzed by TLC and HPLC, and its structures were analyzed by FT-IR, EI-mass and NMR. The dyeing mechanism and fermentation conditions were investigated. Its colour fastness was studied as well. The results obtained are summarized as follows ; The natural indigo powder was dissolved in DMSO and developed in eluent, $CHCl_3/CH_3CN(8.5:1.5v/v)$ by means of TLC for its quality analysis. It was segregated into indirubin as il red colour and indigo as a blue colour. In case of HPLC analysis, the retention times of indirubin and indigo were 7.442 and 6.543, respectively. FT-IR spectrum of indirubin showed a peak for NH residue between 3200 and $3300cm^{-1}.^1H-NMR$ spectrum for indigo displayed AA'BB' spin system caused by indole structure between 6.5 and 7.7ppm of H4, 5, 6 and 7, and -NH proton for indirubin showed an singlet between 10.88 and. 11.0ppm. EI-mass spectrum of indigo an d indirubin both disclosed their molecular size as 262 and it implies that these two substances are isomer.

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Identification of IY81149 and Its Metabolites in the Rat Plasma Using the On-Line HPLC/ESI Mass Spectrometry

  • Myung, Seung-Woon;Min, Hye-Ki;Jin, Chang-Bae;Kim, Myung-Soo;Lee, Seung-Mok;Chung, Gi-Ju;Park, Seong-Jun;Kim, Dong-Yeon;Cho, Hyun-Woo
    • Archives of Pharmacal Research
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    • v.22 no.2
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    • pp.189-193
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    • 1999
  • Reversed-phase high-performance liquid chromatography/mass spectrometry (HPLC/MS) with an eletcrospray ionization (ESI) interface was applied to the identification of metabolites of IY81149 in the rat plasma. Fragments obtained using collision-induced dissociation (CID) in both positive and negative modes were utilized to elucidate the structure of metabolites. The eluent from the conventional HPLC column was split and directly introduced into an ESI-mass spectrometer for the identification of the structures. the CID technique allowed the sensitive identification of sulfonyl-IY81149 and hydroxy-IY81149 from the rat plasma.

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Real-time identification of the separated lanthanides by ion-exchange chromatography for no-carrier-added Ho-166 production

  • Aran Kim;Kanghyuk Choi
    • Journal of Radiopharmaceuticals and Molecular Probes
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    • v.7 no.2
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    • pp.69-77
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    • 2021
  • No-carrier-added holmium-166 (n.c.a 166Ho) separation is performed based on the results of separation conditions using stable isotopes dysprosium (Dy) and holmium (Ho) to minimize radioactive waste from separation optimization procedures. Successful separation of two adjacent lanthanides was achieved by cation-exchange chromatography using a sulfonated resin in the H+ form (BP-800) and α-hydroxyisobutyric acid (α-HIBA) as eluent. For the identification process after separation of stable isotopes, the use of chromogenic reagents alternatively enables on-line detection because the lanthanides are hardly absorb light in the UV-vis region or exhibit radioactivity. Four different chromogenic reagents were pre-tested to evaluate suitable coloring reagents, of which 4-(2-Pyridylazo)resorcinol is the most recommendable considering the sensitivity and specificity for lanthanides. Lanthanide radioisotopes (RI) were monitored for separation with an RI detector using a lab-made separation LC system. Under the proper separation conditions, the n.c.a 166Ho was effectively obtained from a large amount of 100 mg dysprosium target within 2 hrs.

Analysis of Mono-, Di- and Tri-glycerides by high-performance liquid chromatography (HPLC) with evaporative light scattering detection (ELSD) (HPLC/ELSD에 의한 Mono-, Di- 및 Tri-glycerides류 분석)

  • Lee, Man-Ho;Park, Heai-Ku;Kim, In-Whan
    • Analytical Science and Technology
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    • v.19 no.3
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    • pp.189-193
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    • 2006
  • Chromatographic separation of glycerol monostearate, glycerol distearate and glycerol tristearate (GMS, GDS, and GTS) has been performed by normal phase HPLC method utilizing a Zorbax silica ($250{\times}4.6mm$, $5{\mu}m$) column and hexane-hexane, IPA and ethyl acetate mixtures as the eluent within 20 min. The observed reproducibility was less than 5% RSD, Suggesting that ELSD was an effective tool for detection of the glycerol stearates of low volatility without chromophore. The detection limits were in the concentration range of 0.3~2 mg/L, and the calibration curves (the log-log plots) were linear in the range of 4~1000 mg/L (with the slopes of 1.06~1.32). The application of the analytical procedure without pretreatment demonstrated that the proposed chromatographic method would be practical for a routine analysis of commercial products.

Quantitative Analys is of Flavonoids in Hovenia dulcis by Region Using UPLC (UPLC를 이용한 지역별 헛개나무(Hovenia dulcis) 플라보노이드의 정량분석)

  • Dong Hwan Lee;Hyun-Jun Kim
    • Proceedings of the Plant Resources Society of Korea Conference
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    • 2022.09a
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    • pp.100-100
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    • 2022
  • Hovenia dulcis is a herbal plant, which belongs to the Rhamnaceae family and is a native of Japan, China and Korea. Its fruit stalk is called 'Jiguja' in Korea. It has been traditionally used as a medicinal plant in East Asia. It was reported to have detoxification effects on alcohol poisoning, and antioxidant, antidiabetic etc. Sample of 5 g was extracted with 50 mL of 70% EtOH. The supernatant was filtered by 0.45 ㎛ membrane filter before analysis. The UPLC system was performed on Waters alliance UPLC HSS T3 column (2.1 × 100 mm, 1.7 ㎛) with a UV detector. The gradient system was a binary eluent of 0.1% formic acid in water(A) and 0.1% formic acid in acetonitrile(B) with gradient conditions as follows: Initial, 10% B; 1 min, 10% B; 4 min, 20% B; 10 min, 25% B; 12 min, 30% B; 14 min, 90% B; 17 min, 90% B; flow rate of 0.2 mL/min. The samples were injected by 2 µL and were detected at UV 355 nm. As a result of analysis, chromatographic patterns appeared in two cases: samples analyzed for ampelopsin and myricetin, and samples analyzed for taxifolin and quercetin. Among the four compounds, the largest regional difference was found to be taxifolin.

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Studies on Ion-exchange Chromatography of Elements in Special Nonferrous Alloys (비철특수합금에서 금속원소의 이온교환 크로마토그라프에 관한 연구)

  • Kyung Woong Lee;Young Jin Yoo
    • Journal of the Korean Chemical Society
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    • v.29 no.2
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    • pp.178-182
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    • 1985
  • The purpose of this study was to develop a separation method of Zn(II), Cu(II) and Mg(II), by ion exchange chromatography using cation exchange resion (Dowex 50w${\times}$8, 80-100 mesh) and anion exchange (Amberlite IRA-400). Ion exchange resions were packed into 25 ${\times}$ 2cm ID column and flow rate was controlled to 0.30 ml/min. Good eluents for separation of nonferrous metal ions such as Zn(II), Cu(II), Mg(II) were as follow: 0.5M $NaNO_3$ (pH 3.1), 0.2~0.5M HCl + 50~60% Acetone, and 1M HAc + 0.1M NaAcf(pH 3.7) aqueous solution. The mixed solution of 0.1M NaAc(pH 3.7), 0.5M HCl + 50% Acetone were found to be the best eluent for step elution. Analysis of metals were determined by atomic absorption spectrophotometer. In addition, separated Zn(II) fraction was obtained by eluted with 0.12N HCl and 1.5N $NH_4OH$ aqueous solution. This solution was titrated by the E. D. T. A.

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Column Chromatographic Separation of Titanium, Zirconium and Niobium (Ti, Zr 및 Nb의 원통크로마토그라프 분리)

  • Chul Lee;Yung Chang Yim;Koo Soon Chung
    • Journal of the Korean Chemical Society
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    • v.17 no.1
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    • pp.15-19
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    • 1973
  • A method was developed for the separation of titanium, niobium and zirconium together in a group from the coexisting ions of various metals such as iron, cobalt, nickel, yttrium and rare earths by means of the cation exchange column using ${\alpha}$-hydroxyisobutyric acid as the eluent. In the course of the present investigation, it was found that the tailing phenomena of zirconium were attributable to the hydroxide precipitation which was made prior to the elution. For example, if zirconium was precipitated by sodium hydroxide, the tailing of zirconium became very serious in contrast to the results reported by others. This paper describes how these tailing phenomena of zirconium were prevented and how a practical procedure for the separation of these ions was, achieved using ion-exchange method. Using the present method the nuclides of $^{90m}Y$ and $^{90}Y$ were separated with radiochemical purity from the irradiated zirconium.

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Separation of Alkali and Alkaline Earth Metal Ions using Novel HDBPDA Ion Exchanger and Its Ion Exchange Characteristics (새로운 HDBPDA 이온교환체를 사용한 알칼리 및 알칼리토금속 이온들의 분리와 그의 이온교환특성)

  • Kim, Dong-Won;Kim, Chang-Suk;Choi, Ki-Young;Jeon, Young-Shin;Yoon, Yeo-Hag
    • Journal of the Korean Chemical Society
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    • v.37 no.9
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    • pp.820-825
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    • 1993
  • The ion exchange capacity of HDBPDA ion exchanger, {(4,5) : (13,14)-dibenzo-6,9,12-trioxa-3,15,21-triazabicyclo[15.3.l]heneicosa-(1,17,19)(18,20,21) triene ion exchanger: HDBPDA ion exchanger} was 3.8 meq/g. The distribution coefficients of alkali and alkaline earth metal ions in water and the various concentration of hydrochloric acid were determined. Concentration of hydrochloric acid have almost not influenced on the distribution coefficients of alkali and alkaline earth metal ions, but generally, the distribution coefficient was slightly increased with decrease of concentration of hydrochloric acid. The distribution coefficients of metal ions in water are larger than those of various hydrochloric acid concentrations. Also, alkali and alkaline earth metal ions are separated by column ion exchange chromatography using HDBPDA ion exchange with water as eluent. The distribution coefficents of alkali and alkaline earth metal ions were increased with increase of ionic radii of metal ions.

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Use of IMS-RT-PCR for the Rapid Isolation and Detection of Hepatitis A Virus from the Swine Feces (IMS-RT-PCR을 활용한 육성돈 분변으로부터 간염 A형 바이러스의 신속순수분리 및 검출법 연구)

  • Lee, Hee-Min;Kim, Duwoon
    • Korean Journal of Food Science and Technology
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    • v.44 no.5
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    • pp.638-642
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    • 2012
  • Human pathogenic viruses such as hepatitis A and E virus (HAV and HEV), which lead to acute liver failure and death, are foodborne pathogens associated with the consumption of virus-contaminated meats, filter-feeding bivalves, fruits, and salads. Two of the three swine farms examined in this study had HAV and HEV positive stool samples in a nested RT-PCR assay. The use of the immunomagnetic separation (IMS) facilitated the separation of HAV through interactions between the ligand on the virion surface and the antibody from the swine feces containing both HAV and HEV. The nested RT-PCR analysis was performed for the detection of HAV obtained from hepatocarcinoma cell line (PLC/PRF/5) contaminated with eluent fraction of IMS. This indicated that IMS has the potential to simultaneously isolate and concentrate target viruses by changing antibodies linked on the magnetic beads.