• Title/Summary/Keyword: mass-spectrometry

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Structural Study of Oligosaccharides by Low Energy Collision Tandem Mass Spectrometry : Effect of the Acetylation Derivatization (저에너지 충돌 탄뎀 질량분석법을 이용한 올리고당의 연결구조 연구:아세틸화 반응이 미치는 영향)

  • Yoo Yoon, Eun Sun
    • Journal of the Korean Chemical Society
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    • v.42 no.3
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    • pp.297-301
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    • 1998
  • Linkage positions in oligosaccharides may be obtained by FAB CAD MS/MS (Fast Atom Bombardment Collision Activated Dissociation Mass Spectrometry/Mass Spectrometry). Acetylated derivatives of the linkage-isomeric trisaccharides exhibited more useful product ion patterns than the free trisaccharides and provided specific fragmentation patterns according to linkage positions. The reason for the useful linkage dependent spectra patterns of acetylated forms is related to the ability of each linkage in the oligosaccharides to absorb different levels of collision energy and rotational freedom of the individual glycosidic linkage.

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Identification of Degradation Products in the Phosphodiesterase (PDE-4) Inhibitor Roflumilast Using High Resolution Mass Spectrometry and Density Functional Theory Calculations

  • Paul, Saroj Kumar;Dash, Upendra N.
    • Mass Spectrometry Letters
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    • v.6 no.2
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    • pp.38-42
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    • 2015
  • Roflumilast analogs are a group of drugs which act as selective photodiesterase (PDE-4) inhibitor for the treatment severe chronic pulmonary disease associated with chronic brochnonities. Structural identification of degradation products using high resolution mass spectrometry and theoretical investigation by density functional theory have been successfully carried out on roflumilast to identify four degradation products namely, 3,5-dichloropyridin-4-amine, N-(3,5-dichloropyridin-4-yl)-4-(difluoromethoxy)-3-hydroxy benzamide, N-(3,5-dichloropyridin-4-yl)-3-(cyclopropylmethoxy)-4-(difluoromethoxy) benzamide and 3-(cyclopropylmethoxy)-N-(3,5-dichloro-1-oxidopyridin-4-yl)-4-(difluoro methoxy) benzamide, generated in alkali, acidic and oxidative conditions.

Identification of Novel Metabolic Proteins Released by Insulin Signaling of the Rat Hypothalmus Using Liquid Chromatography-Mass Spectrometry (LC-MS)

  • Chin, Chur
    • Journal of Korean Neurosurgical Society
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    • v.42 no.6
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    • pp.470-474
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    • 2007
  • Objective : The brain is dependent on glucose as an energy source. Intricate homeostatic mechanisms have been implicated in maintaining the blood glucose concentration in the brain. The aim of this study is to find the way to identify the metabolic proteins regulating the glucose in rat hypothalamus. Methods : In this study, we analysed the secretome from rat hypothalamus in vivo. We introduced 500 nM of insulin into the rat hypothalamus. The chromatographic patterns of the secretome were identified, after which Mass Spectrometry-Mass Spectrometry (MS-MS) analysis was performed. Results : In Liquid Chromatography-Mass Spectrometry (LC-MS) analysis, 60 proteins were identified in the secretome. Among them, 8 novel proteins were unveiled and were associated with the energy metabolism of insulin signaling in mitochondria of rat hypothalamic neuron. Nineteen other proteins have unknown functions. These ligands were confirmed to be secreting from the rat hypothalmus on insulin signaling by western blotting. Conclusion : The hypothalamus is the master endocrine gland responsible for the regulation of various physiological and metabolic processes. Proteomics using LC-MS analysis offer a efficient means for generating a comprehensive analysis of hypothalamic protein expression by insulin signaling.

General Fragmentations of Alkaloids in Electrospray Ionization Tandem Mass Spectrometry

  • Shim, Hee Jung;Lee, Ji Ye;Kim, Byungjoo;Hong, Jongki
    • Mass Spectrometry Letters
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    • v.4 no.4
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    • pp.79-82
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    • 2013
  • Various types of alkaloids observed in several herbal medicines were analyzed by electrospray ionization tandem mass spectrometry in positive ion mode. In the present study, MS/MS spectralpatterns were investigated for eight-types of alkaloids (aporpine, protoberberine, tetrahydroprotoberberine, benzylisoquinoline, protopine, phthalide, morpine, and bisbenzylisoquinoline). For aporpine- and protoberberine-type alkaloids, main fragmentations occurred at substituted groups on rigid ring structures, not showing ring fusion. Interesting fragmentations due to iminolization and retro-Diels-Alder (RDA) reaction were observed in MS/MS spectra of protopine- and tetrahydroprotobereberine-type alkaloids. Also, several types of fragmentations such as inductive cleavage and ${\alpha}$-cleavage, or bond cleavage between two ring structures were observed depending on their structural characteristics. These fragmentation patterns are expected to allow instant classification of the specific alkaloid type in various MS/MS spectra of alkaloids.

Feasibility of Using Graphite Powder to Enhance Uranium Ion Intensity in Thermal Ionization Mass Spectrometry (TIMS)

  • Park, Jong-Ho
    • Mass Spectrometry Letters
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    • v.7 no.4
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    • pp.102-105
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    • 2016
  • This study explored the feasibility of using a carburization technique to enhance the ion intensity of isotopic analysis of ultra-trace levels of uranium using thermal ionization mass spectrometry (TIMS). Prior to fixing uranium samples on TIMS filaments, graphite powder suspended in nitric acid was deposited on rhenium filaments. We observed an enhancement of $^{238}U^+$ intensity by a factor of two when carburization was used, and were able to roughly optimize the amount of graphite powder necessary for carburization. The positive shift in heating current when evaporating filaments upon carburization implies that uranium was chemically altered by carburization, when compared to normal fixation processes. The good agreement between our method and known standards down to an ultra-trace level shows that the proposed technique can be applied to isotopic uranium analysis down to abundances of ~10 pg.

Determination of the Concentration and Isotope Ratio of Uranium in Soil and Water by Thermal Ionization Mass Spectrometry

  • Park, Jong-Ho;Park, Sujin;Song, Kyuseok
    • Mass Spectrometry Letters
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    • v.5 no.1
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    • pp.12-15
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    • 2014
  • Thermal ionization mass spectrometry (TIMS) was used to determine the concentration and isotope ratio of uranium contained in samples of soil and groundwater collected from Korea. Quantification of uranium in ground water samples was performed by isotope dilution mass spectrometry. A series of chemical treatment processes, including chemical separation using extraction chromatography, was applied to the soil samples to extract the uranium. No treatments other than filtration were applied to the groundwater samples. Isotopic analyses by TIMS showed that the isotope ratios of uranium in both the soil and water samples were indistinguishable from those of naturally abundant uranium. The concentration of uranium in the groundwater samples was within the U.S. acceptable standards for drinking water. These results demonstrate the utility of TIMS for monitoring uranium in environmental samples with high analytical reliability.

Electron Capture Dissociation Mass Spectrometry for Gaseous Protonated Melittin Ions and Its Single Amino Acid Substituted Variants

  • Yu, Seonghyun;Jang, Hwa-yong;Oh, Han Bin
    • Mass Spectrometry Letters
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    • v.10 no.4
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    • pp.117-122
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    • 2019
  • This study demonstrated the sensitivity of electron capture dissociation mass spectrometry (ECD-MS) to probe subtle conformational changes in gaseous melittin ions induced by the substitution of an amino acid. ECD-MS was performed for triply and quadruply-protonated melittin and its variants obtained by a single amino acid substitution, namely, D-Pro14, Pro14Ala, and Leu13Ala. Although native triply-protonted melittin showed only a few peptide backbone cleavage products, the D-Pro14 and Pro14Ala variants exhibited extensive backbone fragments, suggesting the occurrence of a significant structural or conformational change induced by a single amino acid substitution at Pro14. On the contrary, the substitution at Leu13, namely Leu13Ala (+3), did not cause significant changes in the ECD backbone fragmentation pattern. Thus, the sensitivity of ECD-MS is demonstrated to be good enough to probe the aforementioned conformational change in melittin.

Quantification of Three Prohibited Anabolic-Androgenic Steroids in Equine Urine using Gas Chromatography-Tandem Mass Spectrometry

  • Young Beom Kwak;Shaheed Ur Rehman;Hye Hyun, Yoo
    • Mass Spectrometry Letters
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    • v.14 no.3
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    • pp.104-109
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    • 2023
  • Anabolic-androgenic steroids (AAS) are used illegally to enhance muscle development and increase strength and power. In this study, a reliable, and sensitive quantitative method was developed and validated using heptafluorobutyric acid anhydride (HFPA) derivatives for the simultaneous detection of prohibited AAS (testosterone [TS], boldenone [BD], 5α-estrane-3β,17α-diol [EAD]) using gas chromatography-tandem mass spectrometry (GC-MS/MS). For processing the samples, solid phase extraction, methanolic hydrolysis, and liquid-liquid extraction were used. For detection using mass spectrometry, the multiple reaction monitoring (MRM) mode was used with the electron ionization (EI) positive mode. The method was evaluated for selectivity, linearity, lower limit of quantification, intra- and inter-day precision, accuracy, and stability. The results showed that the method was accurate and reproducible for the quantitation of the three steroids. The developed method was finally applied to the analysis of a suspect gelding urine sample received from the Asian Quality Assurance Program (AQAP).

Recent Developments in Nuclear Forensic and Nuclear Safeguards Analysis Using Mass Spectrometry

  • Song, Kyuseok;Park, Jong-Ho;Lee, Chi-Gyu;Han, Sun-Ho
    • Mass Spectrometry Letters
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    • v.7 no.2
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    • pp.31-40
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    • 2016
  • The analysis of nuclear materials and environmental samples is an important issue in nuclear safeguards and nuclear forensics. An analysis technique for safeguard samples has been developed for the detection of undeclared nuclear activities and verification of declared nuclear activities, while nuclear forensics has been developed to trace the origins and intended use of illicitly trafficked nuclear or radioactive materials. In these two analytical techniques, mass spectrometry has played an important role in determining the isotope ratio of various nuclides, contents of trace elements, and production dates. These two techniques typically use similar analytical instruments, but the analytical procedure and the interpretation of analytical results differ depending on the analytical purpose. The isotopic ratio of the samples is considered the most important result in an environmental sample analysis, while age dating and impurity analysis may also be important for nuclear forensics. In this review, important aspects of these techniques are compared and the role of mass spectrometry, along with recent progress in related technologies, are discussed.

Change of MS Method and Comparison of SIFT-MS Method

  • CHOI, Jong-Sun;KWON, Lee-Seung;LEE, Ji-Hoon;KIM, Romertta;KWON, Woo-Taeg
    • Journal of Wellbeing Management and Applied Psychology
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    • v.5 no.1
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    • pp.37-46
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    • 2022
  • Purpose: This study examines the history of the evolution of MS analysis and intends to consider the future direction of technological development through the difference from the latest technology, SIFT-MS. Research design, data and methodology: A method of analysis will be described in detail at the below by SIFT-MS (Selected Ion Flow Mass Spectrometry), which is a technology developed by a company called SIFT Technologies. Results: The initial concept of mass spectrometry was begun in the late 1890s, and it continues to evolve even after the 21st century through the ripening stage of the 20th century. The development process of mass spectrometry by year has been described in detail in the Main text. Conclusions: Mass spectrometry, qualitative and quantitative analysis of substances plays a very important role in the research and medical fields. The development of these analytical methods is expected to continue in the future, and faster and more accurate qualitative analysis and mass spectrometry will be developed than the level currently reached. In addition, it is expected that hardware and software will be configured so that non-analysis experts can handle it easily, and it will be used as a technology that is more closely related to our lives.