• Title/Summary/Keyword: Liquid Chromatography

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On the Pyrolysis of Polymers III. Identification of Gases from Rubber Pyrolysis by Gas Chromatography (高分子物質의 熱分解에 關한 硏究 (第3報) 合成고무類의 熱分解生成物의 Gas Chromatography에 의한 檢索과 合成고무 確認에의 利用)

  • Chwa-Kyung Sung
    • Journal of the Korean Chemical Society
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    • v.7 no.2
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    • pp.115-121
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    • 1963
  • Aliphatic hydrocarbon gases from rubber pyrolysis have been identified by gas chromatography with tetraethyleneglycol dimethylether column. Rubbers used in this work are polyisoprene, SBR, NBR, polybutadiene, buthyl rubber, polychloroprene and polyurethane rubber. The chromatogram is characteristic for each polymer. Author proposes a method of identification of synthetic rubbers by gas chromatograph of pyrolyzed gas. Sample is pyrolyzed at $450^{\circ}C$ under nitrogen or more effectively helium and gaseous portion, which eliminated liquid condensate, is passed to the column. The appearance of exclusively large peak of isoprene, isobutylene and carbon dioxide shows the presence of polyisoprene, polyisobutylene and polyurethane, respectively. Large peak of butadiene will appear in case of polybutadiene, SBR and NBR, but SBR can be identified through the styrene peak in gas chromatogram of liquid pyrolyzate and NBR can be identified by the evolution of hydrogen cyanide during pyrolysis. Polychloroprene is identified by the evolution of hydrogen chloride. This method could be applied to the identification of copolymer or polymer blend.

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Identification of Actinomycins by High Performance Liquid Chromatography and Fast Atom Bombardment Mass Spectrometry

  • Cho, Seong-Eun;Goo, Yang-Mo;Kim, Kyoung-Ja
    • Archives of Pharmacal Research
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    • v.17 no.6
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    • pp.424-427
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    • 1994
  • An acinomycin complex isolated from culture broth of a soil microorganism, SNUS 9305-011 has been examined by High performance liquid chromatography (HPLC). From the analysis of the fractions obtained by column chromatography of the ethyl acetate extract, three actinomycin components are confimed . The HPLC analysis is carried out with a CN-bonded nucleosil column. Comparison of the retention times of the components with those of actinomycin D, C complex, $X_{o{\beta}$, and V and suggests that they are different actinomycins. FBA mass spectra fo the coponents also shows different molecular ions from those of standards and other reported actionbmycins. The present work has demonstrated that actinomycin components can be separated by a CN-bonded HPLC column, and that ocmparison of their HPLC chormatograms with authentic smaples and information on their molecular ions can be successfully employed for indentification of actionmycins.

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Determination of Fluorescent Whitening Agents in Paper Materials by Ion-Pair Reversed-Phase High-Performance Liquid Chromatography

  • Kim, Jeong Soo;Kim, Do Hwan;Kim, Keon
    • Bulletin of the Korean Chemical Society
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    • v.33 no.12
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    • pp.3971-3976
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    • 2012
  • A simple method was developed for the analysis of seven stilbene-type fluorescent whitening agents (FWAs) in paper materials by ion-pair reversed-phase high-performance liquid chromatography with fluorescence detection. These stilbene-type FWAs included two disulfonate, two tetrasulfonate, and three hexasulfonate compounds. After optimization of chromatographic conditions, the FWAs were satisfactorily separated using a reversed-phase column (RP-18) with the following isocratic mobile phase: methanol-water (60:40) containing 17.5 mM TBABr and 10 mM citrate buffer (pH = 7.0). The calibration plot was linear in the range from 5 to 500 ng/mL for two disulfo-FWAs and from 1 to 500 ng/mL for the other five FWAs. Precision levels of the calibration curve as indicated by RSD of response factors were 1.2 and 8.1%. Limits of quantitation (LOQ) ranged from 1.2 to 11 ng/mL.

Sterol Compositions in Some Cucurbitaceae Vegetable Oils (몇가지 박과 식물 종자유중의 Sterol 조성)

  • Tae Myoung Jeong;Min Suk Yang;Taro Matsumoto
    • Journal of the Korean Chemical Society
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    • v.21 no.3
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    • pp.193-203
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    • 1977
  • Three sterol fractions; 4-desmethyl-, 4-monomethyl-, and 4,4-dimethylsterol, separated by thin layer chromatography from the unsaponifiables of five Cucurbitaceae (cucumber, watermelon, sponge cucumber, gourd and snake gourd) seed oils were analyzed by gas liquid chromatography and combined gas liquid chromatography-mass spectrometry. ${\alpha}$-Spinasterol, ${\Delta}^{7,22,25}$-stigmastatrienol and ${\Delta}^{7,25}$-stigmastadienol isolated from the 4-desmethylsterol fraction were identified by IR, NMR and mass spectrometry.

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Studies on the Sterol Components of Torreya Nut of Korea (한국산 비자중의 스테롤 성분에 관한 연구)

  • 정보섭;고영수
    • YAKHAK HOEJI
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    • v.22 no.2
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    • pp.87-90
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    • 1978
  • "Bija"(Torreya nut), a tree belonging to the Torreyaceae family, is cultivated in Jae Joo Do and Jun Ra Do, Korea. The seed of Torreya nucifera, which has been widely used as folkmedicine in the treatment of tapeworm infestation, was examined on the sterol composition determined by gas liquid chromatography and thin layer chromatography on the preparative plates. Sterols were obtained from the nonsaponifiable matters of ether extract of the seed. It was noted that .betha.-sitosterol was the major sterol in the nut. The results showed that contents of sterols were campesterol 3.15-3.75%, stigmasterol 5.38-5.67%, $\beta$-sitosterol 85.61-86.28% and ${\delta}^{7}$-sterol 4.91-5.19% by gas liquid chromatography.

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Isolation of a Calcium-binding Peptide from Chlorella Protein Hydrolysates

  • Jeon, So-Jeong;Lee, Ji-Hye;Song, Kyung-Bin
    • Preventive Nutrition and Food Science
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    • v.15 no.4
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    • pp.282-286
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    • 2010
  • To isolate a calcium-binding peptide from chlorella protein hydrolysates, chlorella protein was extracted and hydrolyzed using Flavourzyme, a commercial protease. The degree of hydrolysis and calcium-binding capacity were determined using trinitrobenzenesulfonic acid and orthophenanthroline methods, respectively. The enzymatic hydrolysis of chlorella protein for 6 hr was sufficient for the preparation of chlorella protein hydrolysates. The hydrolysates of chlorella protein were then ultra-filtered under 5 kDa as molecular weight. The membrane-filtered solution was fractionated using ion exchange, reverse phase, normal phase chromatography, and fast protein liquid chromatography to identify a calcium-binding peptide. The purified calcium-binding peptide had a calcium binding activity of 0.166 mM and was determined to be 700.48 Da as molecular weight, and partially identified as a peptide containing Asn-Ser-Gly-Cys based on liquid chromatography/electrospray ionization tandem mass spectrum.

New Polyacetylene Compounds from Panax Ginseng C. A. Meyer$^\dag$

  • Shim, Sang-Chul;Chang, Suk-Ku;Hur, Chan-Woo;Kim, Chang-Kew
    • Bulletin of the Korean Chemical Society
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    • v.8 no.4
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    • pp.272-275
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    • 1987
  • Two polyacetylene compounds having diyn-ene chromophore were isolated from fresh Korean ginseng roots through solvent fractionation, partition and silica gel column chromatography. The low pressure semi-preparative liquid chromatography and high performance preparative liquid chromatography were used for final separation of polyacetylenic fractions. The chemical structures of these polyacetylenes were determined to be heptadeca-1,8-dien-4,6-diyn-3,10-diol and heptadeca-1,4-dien-6,8-diyn-3,10-diol by UV, FT-IR, $^1H\;NMR,\;^{13}C\;NMR,$ mass spectra and elemental analysis.

Purification of the Candida utilis Extracellular Invertase using Affinity Chromatography

  • Ginalska, G.;Belcarz, A.;Lobarzewski, J.;Leonowicz, A.;Cho, Nam-Seok
    • Journal of the Korean Wood Science and Technology
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    • v.30 no.3
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    • pp.12-17
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    • 2002
  • The extracellular invertase (EC 3.2.1.26) (Candida utilis) preparation was obtained from the liquid medium after desalting and freeze drying. This prepared enzyme was used for the comparative purification on 4 activated matrices by liquid column affinity chromatography method. In this method there were used controlled porous glass (CPG) silanized covalently activated by keratin, silanized silica gel and silica gel covalently covered by keratin. It was found that the invertase purification process was better using both CPG matrices (silanized CPG and keratin activated CPG) than these with two silica gel supports. Also the elution coefficient of the invertase from the two CPG columns was about 93 to 94%. Two silica gel supports found to be superior in terms of purification efficiency. The invertase purification process was confirmed by PAGE electrophoresis.

UHPLC System Shutdown and Reactivation Advice (UHPLC 시스템 종료 및 재가동 시 가이드)

  • Mark Fever;Gemma Lo
    • FOCUS: LIFE SCIENCE
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    • no.1
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    • pp.8.1-8.3
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    • 2024
  • Ultra-high performance liquid chromatography (UHPLC) systems are integral to modern analytical laboratories, necessitating careful maintenance and operation protocols to ensure optimal performance. This document provides comprehensive guidelines for the proper shutdown and reactivation of UHPLC systems to prevent damage and maintain operational efficiency. • Shutdown: Remove the column and replace it with a union to avoid blockages. Flush the system with a compatible solvent mix, clean mobile phase reservoirs to prevent microbial growth, flush the pump with storage solvent, and clean the autosampler, including the needle and injection port. • Reactivation: Inspect the system for wear or damage, gradually reintroduce mobile phases starting with a weak solvent, reinstall the column securely, and perform system checks on baseline stability, pressure consistency, and detector performance. By adhering to these guidelines, laboratories can ensure the longevity and reliability of their UHPLC systems, maintaining high analytical performance and minimizing downtime. These procedures help prevent common issues such as blockages, contamination, and component wear, thereby supporting efficient and accurate analytical operations.

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A New Analytical Method for Erythromycin in Fish by Liquid Chromatography/Tandem Mass Spectrometry

  • Park, Mi-Jung;Park, Mi-Seon;Lee, Tae-Seek;Shin, Il-Shik
    • Food Science and Biotechnology
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    • v.17 no.3
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    • pp.508-513
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    • 2008
  • Erythromycin has been used to treat Streptococosis, Edwardsiel1osis, Vibriosis, Bacterial enteritis in the cultured fish. In this study, a rapid and effective erythromycin analysis method with new sample treatment protocol and liquid chromatography/tandem mass spectrometry (LC/MS/MS) system for fish products was developed. For the erythromycin extraction from fish muscle, the solvent mixture composed of 0.2% meta-phosphoric acid and methanol (6:4) showed good recovery rate, and the optimum extraction solvent volume was 20 mL. Erythromycin detection using LC/MS/MS were carried out under electro spray ionization (ESI) positive condition and erythromycin mass value 576.2 and 157.9. And the detection limit of the established method was 0.005 mg/kg in fish products. The recovery rate of the developed method applied to the fish species were as following, olive flounder, $87.6{\pm}5.0%$; black rockfish, $87.2{\pm}6.4%$; eel, $85.2{\pm}4.8%$; and rainbow trout, $86.0{\pm}6.2%$. In the established method in this study, the correlation of coefficient values ($R^2$) of erythromycin calibration curve (n=11) was 0.9998.