• Title/Summary/Keyword: ESI-MS

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Simultaneous determination of aminoglycoside antibiotics by HPLC/MS (HPLC/MS을 이용한 aminoglycoside 항생제 동시 분석에 관한 연구)

  • Roh, Young-Sun;Baek, Gui-Jung;Kim, Seung-Yong;Choi, Eun-Young;Seo, Heyng-Seok;Hur, Boo-Hong;Joung, Dong-Suk
    • Korean Journal of Veterinary Service
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    • v.30 no.1
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    • pp.1-12
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    • 2007
  • A liquid chromatographic method has been developed for the analysis of aminoglycoside antibiotics (AMGs) using Heptafluorobutyric acid (HFBA) as a ion-pairing reagent. AMGs (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygrosin B, kanamycin, neomycin, spectinomycin and tobramycin) were formed by reaction with HFBA as ion-pairing reagent. HFBA was attached to corresponding amino group of AMGs. These AMGs compounds were separated and detected by electrospray ionization mass spectrometry (ESI-MS). The experimental conditions for separation of AMGs were optimized and validated. A simple liquid chromatographic method for the determination of AMGs was demonstrated.

Intensive Proteomic Approach to Identify Secreted Peptides/Proteins from 3T3-L1 Adipocytes using Gel Electrophoresis and Liquid Chromatograph Separation Methods (젤 전기영동 및 액체 크로마토그래피 분리 방법을 이용하여 지방 세포로부터 분비되는 단백질들에 대한 프로테오믹스 연구 방법)

  • Hwang, Hyun-Ho;Baek, Moon-Chang
    • YAKHAK HOEJI
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    • v.55 no.3
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    • pp.203-212
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    • 2011
  • Adipocytes have been known to secrete a number of important proteins called adipokines with roles in energy metabolism, reproduction, cardiovascular function and immunity. In this study we have attempted to identify intensively secretory proteins from 3T3-L1 adipocytes. 3T3-L1 preadipocytes were differentiated into mature adipocytes and then the cells were left in serum-free medium. The supernatant was filtrated and dialyzed. Lyophilized secretome was fractionated by two different methods, 1-D SDS PAGE and RP-FPLC. The tryptic peptides from the gel slices and the FPLC fractions were analyzed by nanoLC/ESI-MS/MS. We identified a total of 303 identical proteins from two methods, 251 proteins from 1-D gel and 184 proteins from RP-FPLC. 86 of them were listed as a secretory protein Finally, we identified many known or unknown secreted proteins existed in the low level including adiponectin, angiotensinogen, bone morphogenetic protein-1 (BMP-1), macrophage migration inhibitory factor (MIF), insulin like growth factor-II (IGF-II), interleukin-6 (IL-6), follistatin-related protein-1, minecan, and resistin. The existence of some of secreted proteins has been confirmed in RNA level. This proteomic experiment is useful for the intensive screening of secretory proteins in many kinds of other cells.

Hydrolysis of Penicillin G and Carbenicillin in Pure Water - As Studied by HPLC/ESI-MS

  • Kolek, Marta;Franski, Rafal;Franska, Magdalena
    • Mass Spectrometry Letters
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    • v.10 no.4
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    • pp.108-111
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    • 2019
  • The hydrolysis of penicillin G, carbenicillin and ampicillin in pure water at room temperature was studied by high pressure liquid chromatography electrospray ionization mass spectrometry. Hydrolysis of ampicillin did not occur under these conditions; however, penicillin G and carbenicillin were completely hydrolyzed after seven days. A short interpretation of this difference is proposed. The mass spectrometric behaviour, namely ESI response and fragmentation pathway, of hydrolyzed penicillin G and hydrolyzed carbenicillin have been also discussed.

Hydroxylation of Resveratrol with DoxA In Vitro: An Enzyme with the Potential for the Bioconversion of a Bioactive Stilbene

  • Rimal, Hemraj;Yu, Sang-Cheol;Lee, Joo-Ho;Yamaguchi, Tokutaro;Oh, Tae-Jin
    • Journal of Microbiology and Biotechnology
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    • v.28 no.4
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    • pp.561-565
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    • 2018
  • The late-stage doxorubicin biosynthesis pathway acting enzyme (DoxA) from Streptomyces peucetius CYP129A2 exhibited substrate promiscuity towards the stilbene group of compounds such as resveratrol. DoxA along with two accessory enzymes ferrdoxin reductase and ferredoxin from spinach hydroxylated resveratrol at the 3'-position in vitro to produce piceatannol. The product was identified by HPLC-PDA and high-resolution HR-qTOF-ESI/MS analyses in positive mode. The ESI/MS fragments resembled the hydroxylated product of resveratrol.

Applications of Tandem Mass Spectrometry in the Structure Determination of Permethylated Sialic Acid-containing Oligosaccharides

  • Yoo, Eun-Sun;Yoon, In-Mo
    • Bulletin of the Korean Chemical Society
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    • v.26 no.9
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    • pp.1347-1353
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    • 2005
  • Sets of sialic acid-containing trisaccharides having different internal and terminal linkages have been synthesized to develop a sensitive method for analysis of the reducing terminal linkage positions. The trisaccharides, sialyl($\alpha$ 2-3)Gal($\beta$ 1-3)GalNAc and sialyl($\alpha$ 2-3)Gal($\beta$ 1-X)GlcNAc where X=3, 4 and 6, were synthesized and examined using electrospray ionization (ESI)-collision induced dissociation (CID) tandem mass spectrometry (MS/MS). The compounds chosen for this study are related to terminal groups likely to be found on polylactosamine-like glycoproteins and glycolipids which occur on the surface of mammalian cells. The purpose of this study is to develop tandem mass spectrometral methods to determine detailed carbohydrate structures on permethylated or partially methylated oligosaccharides for future applications on biologically active glycoconjugates and to exploit a faster method of synthesizing a series of structural isomeric oligosaccharides to be used for further mass spectrometry and instrumental analysis.

Chemical Investigation of the Constitutive Flavonoid Glycosides of the Leaves of Crataegus sinaica

  • El-Mousallamy, Amani M. D.
    • Natural Product Sciences
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    • v.4 no.2
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    • pp.53-57
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    • 1998
  • Leaves of Crataegus sinaica Boiss, contain the new C-glycosyl flavone $3"',4”’-di-O-acetyl-2“-O-{\alpha}-rhamnosylvitexin$, together with the hitherto unknown, dihydroflavonol 3-O-xyloside, (2R:3R)-dihydroquercetin-$3-O-{\beta}-xylopyranoside$. The known compounds (+)-catechin, (-)-epicatechin, vicenin-II, $2"-O-{\alpha}-rhamnosylvitexin$, and $4"'-O-acetyl-2"-O-{\alpha}-rhamnosylvitexin$ were also characterized. Structures were established by conventional methods of analysis and confirmed by $^1H-,\;^{13}C-NMR$, and ESI-MS.

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Identification of Ceftiofur Oxidation Products by High-Performance Liquid Chromatography/Electrospray Ionization/Tandem Mass Spectrometry

  • Lim, Young-Hee;Park, Deok-Hie;Youn, Yeu-Young;Kim, Kyung-Hoon;Cho, Hye-Sung
    • Mass Spectrometry Letters
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    • v.2 no.1
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    • pp.16-19
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    • 2011
  • Oxidation products of ceftiofur were formed in hydrogen peroxide solution. The structures of the ceftiofur oxidation products were characterized by high-performance liquid chromatography/electrospray ionization/tandem mass spectrometry (HPLC/ESI/MS/MS). The products were identified as compounds oxidized at the sulfur of a cephem ring. For further analysis, experiments were performed using $O^{18}$-labeled hydrogen peroxide. In addition, density-functional calculations were carried out for six possible oxidation products to support the experimental results.

Unique Phenolic Sulphate Conjugates from the Flowers of Tamarix amplexicaulis

  • Souleman, Ahmed A.M.;Barakat, Heba H.;Hussein, Sahar A.M.;El-Mousallamy, Amani M.D.;Nawwar, Mahmoud A.M.
    • Natural Product Sciences
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    • v.4 no.4
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    • pp.245-252
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    • 1998
  • The unique sulphated phenolics, gallic acid 3-methyl ether 5-potassium sulphate, isoferulic acid 3-potassium sulphate, and ellagic acid 4,4'-dimethyl ether 3-potassium sulphate have been isolated from the flowers of Tamarix amplexicaulis Ehrenb. (Tamaricaceae). The hitherto unknown natural phenolic acid, gallic acid 3-methyl ether, together with the known phenolic, gallic acid, gallic acid 4-methyl ether, isoferulic acid, ferulic acid, ellagic acid, and ellagic acid 4,4'-dimethyl ether have been also separated and characterized. The structures were established by conventional methods, including electrophoretic analysis and confirmed by ESI-MS, $^1H-\;and\;^{13}C-NMR$.

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