• Title/Summary/Keyword: Ionization development

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Fragmentation Behavior Studies of Chalcones Employing Direct Analysis in Real Time (DART)

  • Motiur Rahman, A.F.M.;Attwa, Mohamed W.;Ahmad, Pervez;Baseeruddin, Mohammad;Kadi, Adnan A.
    • Mass Spectrometry Letters
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    • v.4 no.2
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    • pp.30-33
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    • 2013
  • Chalcones are naturally occurring, biologically active molecules generating interest from a wide range of research applications including synthetic methodology development, biological activity investigation and studying fragmentation patterns. In this article, a series of chalcones has been synthesized and their fragmentation behavior was studied using modern ambient ionization technique Direct Analysis in Real Time (DART). DART ion source connected with an ion trap mass spectrometer was used for the fragmentation of various substituted chalcones. The chalcones were introduced to the DART source using a glass capillary without sample preparation step. All the chalcones showed prominent molecular ion peaks $[M]^{{\cdot}+}$ corresponding to the structures. Multistage mass spectral data $MS^n$ ($MS^2$ and $MS^3$) were collected for all the chalcones studied. The chalcones with substitutions at 3, 4 or 5 positions gave product ion peaks with the loss of a phenyl radical ($Ph^{\cdot}$) by radical initiated ${\alpha}$-cleavage, while substitution at 2 position of chalcone in the A-ring gave a product ion peak with the loss of substituted styryl radical (PhCH = $CH^{\cdot}$). In case of the chalcones with the substituent at 4 positions in A and B rings gave both types of fragmentation patterns. In conclusion, chalcones can be easily characterized using modern DART interface in very short time and efficiently without any cumbersome sample pretreatment.

Comprehensive proteome analysis using quantitative proteomic technologies

  • Kamal, Abu Hena Mostafa;Choi, Jong-Soon;Cho, Yong-Gu;Kim, Hong-Sig;Song, Beom-Heon;Lee, Chul-Won;Woo, Sun-Hee
    • Journal of Plant Biotechnology
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    • v.37 no.2
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    • pp.196-204
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    • 2010
  • With the completion of genome sequencing of several organisms, attention has been focused to determine the function and functional network of proteins by proteome analysis. The recent techniques of proteomics have been advanced quickly so that the high-throughput and systematic analyses of cellular proteins are enabled in combination with bioinformatics tools. Furthermore, the development of proteomic techniques helps to elucidate the functions of proteins under stress or diseased condition, resulting in the discovery of biomarkers responsible for the biological stimuli. Ultimate goal of proteomics orients toward the entire proteome of life, subcellular localization, biochemical activities, and their regulation. Comprehensive analysis strategies of proteomics can be classified as three categories: (i) protein separation by 2-dimensional gel electrophoresis (2-DE) or liquid chromatography (LC), (ii) protein identification by either Edman sequencing or mass spectrometry (MS), and (iii) quanitation of proteome. Currently MS-based proteomics turns shiftly from qualitative proteome analysis by 2-DE or 2D-LC coupled with off-line matrix assisted laser desorption ionization (MALDI) and on-line electrospray ionization (ESI) MS, respectively, to quantitative proteome analysis. Some new techniques which include top-down mass spectrometry and tandem affinity purification have emerged. The in vitro quantitative proteomic techniques include differential gel electrophoresis with fluorescence dyes, protein-labeling tagging with isotope-coded affinity tag, and peptide-labeling tagging with isobaric tags for relative and absolute quantitation. In addition, stable isotope labeled amino acid can be in vivo labeled into live culture cells through metabolic incorporation. MS-based proteomics extends to detect the phosphopeptide mapping of biologically crucial protein known as one of post-translational modification. These complementary proteomic techniques contribute to not only the understanding of basic biological function but also the application to the applied sciences for industry.

Pentafluorophenylprophyl Ligand-based Liquid Chromatography-Tandem Mass Spectrometric Method for Rapid and Reproducible Determination of Metformin in Human Plasma

  • Yang, Jeong Soo;Oh, Hyeon Ju;Jung, Jin Ah;Kim, Jung-Ryul;Kim, Tae-Eun;Ko, Jae-Wook;Lee, Soo-Youn;Huh, Wooseong
    • Bulletin of the Korean Chemical Society
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    • v.34 no.11
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    • pp.3284-3288
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    • 2013
  • This paper describes first development and validation of pentafluorophenylprophyl ligand-based liquid chromatography coupled to tandem mass spectrometry (PFPLC-MS/MS) method to determine metformin, a highly polar compound, in human plasma. Metformin and Phenformin (internal standard) were extracted from human plasma 50 ${\mu}L$ with a single-step protein precipitation. The chromatographic separation was performed using a linear gradient elution of mobile phase involving 5.0 mM ammonium formate solution with 0.1% formic acid (A) and acetonitrile (B) over 3.0 min of run time on a Phenomenex Luna PFP column. The detection was performed using a triple-quadrupole tandem mass spectrometer (Waters Quattro micro) with electrospray ionization in the mode of positive ionization and multiple-reaction monitoring (MRM). The developed method was validated with 5.0 ng/mL of lower limit of quantification (LLOQ). The calibration curve was linear over 5-3000 ng/mL of the concentration range ($R^2$ > 0.99). The specificity, selectivity, carry-over effect, precision, accuracy and stability of the method met the acceptance criteria. The method developed in this study had had rapidness, simplicity and ruggedness. The reliable method was successfully applied to high throughput analysis of real samples for a practical purpose of a pharmacokinetic study.

Development of chemical ionization method in a GC-TOF mass spectrometer for accurate mass and isotope ratio measurement (Accurate mass 및 isotope ratio 측정을 위한 GC-TOF 질량분석기에서의 화학적 이온화방법)

  • Chung, Joo-Hee;Na, Yun-Cheol;Hwang, Geum-Sook;Shin, Jeoung-Hwa;Ahn, Yun-Gyong
    • Analytical Science and Technology
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    • v.24 no.1
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    • pp.15-23
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    • 2011
  • An accurate mass and isotope ratio were determined using a gas chromatography/time of flight mass spectrometer in CI positive mode for the identification of unknown metabolites. High mass tune was used to improve the ion intensity of $[M+H]^+$. Chromatographic resolution and dynamic range enhancement were performed to obtain more reliable accurate masses and correct isotope abundance ratios. Average absolute errors of mass and isotope ratios for 24 reference metabolite -TMS (trimethylsilyl) derivatives were 6.8 ppm, 1.5% of (M+1/M ratio) and 1.7% of (M+2/M ratio), respectively. The correct formulas of twenty one compound were retrieved within top-2 hit from the heuristic algorithm for elemental composition using each accurate mass and isotope abundance ratio.

Development of Analytic Methods for Veterinary Drug Residue in Animal Products by Liquid Chromatography-Mass Spectrometry (축산물 중 잔류 성장보조제 분석을 위한 액체크로마토그라피-질량분석법 개발 및 적용)

  • Lee, Soo Hyun
    • Journal of Convergence for Information Technology
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    • v.11 no.2
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    • pp.107-116
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    • 2021
  • In this study, an analytical method was developed for estradiol-17��, testosterone, and progesterone, which are growth promoters as veterinary drug residues in animal food. The analytes were separated using liquid chromatography, and was injected into a mass spectrometer through the electrospray ionization(ESI) process and detected in multiple reaction monitoring(MRM) mode. As the method was validated by CODEX CAC/GL 71-2009 guideline, it met the acceptable. The analysis of beef, pork, and chicken distributed in Korea was conducted with an established method to confirm the applicability of the actual sample. It was confirmed that the developed method can be quickly and reliably in the analysis for the growth promoters identified in domestic distributed livestock products. Through subsequent research, a highly utilized analysis method will be completed if the number of growth promoters is expanded based on the method and the simultaneous analytical method is established by including all of it.

Determination of N-nitrosodimethylamine in zidovudine using high performance liquid chromatography-tandem mass spectrometry

  • Yujin Lim;Aelim Kim;Yong-Moon Lee;Hwangeui Cho
    • Analytical Science and Technology
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    • v.36 no.6
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    • pp.281-290
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    • 2023
  • Zidovudine is an antiretroviral agent prescribed for the prevention and treatment of human immunodeficiency virus/acquired immune deficiency syndrome (HIV/AIDS). It is typically recommended to be used in combination with other antiretroviral drugs. Zidovudine has the potential to generate N-nitrosodimethylamine (NDMA) in the presence of dimethylamine and nitrite salt under acidic reaction conditions during the drug manufacturing process. NDMA is a potent human carcinogen that may be detected in drug substances or drug products. An analytical method was developed to determine NDMA in pharmaceuticals including zidovudine using high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The analysis involved reversed-phase chromatography on a Kinetex F5 column with a mobile phase comprising water-acetonitrile mixtures. The detection of positively charged ions was conducted using atmospheric pressure chemical ionization (APCI). The calibration curve demonstrated excellent linearity (r = 0.9997) across the range of 1-50 ng/mL with a highly sensitive limit of detection (LOD) at 0.3 ng/mL. The developed method underwent thorough validation for specificity, linearity, accuracy, precision, robustness, and system suitability. This sensitive and specific analytical method was applied for detecting NDMA in zidovudine drug substance and its formulation currently available in the market, indicating its suitability for drug quality management purposes.

Potential Importance of Proteomics in Research of Reproductive Biology (생식생물학에세 프로테오믹스의 응용)

  • Kim Ho-Seung;Yoon Yong-Dal
    • Development and Reproduction
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    • v.8 no.1
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    • pp.1-9
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    • 2004
  • The potential importance of proteomic approaches has been clearly demonstrated in other fields of human medical research, including liver and heart disease and certain forms of cancer. However, reproductive researches have been applied to proteomics poorly. Proteomics can be defined as the systematic analysis of proteins for their identity, quantity, and function. It could increase the predictability of early drug development and identify non-invasive biomarkers of toxicity or efficacy. Proteome analysis is most commonly accomplished by the combination of two-dimensional gel electrophoresis(2DE) and MALDI-TOF(matrix-assisted laser desorption ionization-time of flight) MS(mass spectrometry) or protein chip array and SELDI-TOF(surface-enhanced laser desorption ionization-time of flight) MS. In addition understanding the possessing knowledge of the developing biomarkers used to assess reproductive biology will also be essential components relevant to the topic of reproduction. The continued integration of proteomic and genomic data will have a fundamental impact on our understanding of the normal functioning of cells and organisms and will give insights into complex cellular processes and disease and provides new opportunities for the development of diagnostics and therapeutics. The challenge to researchers in the field of reproduction is to harness this new technology as well as others that are available to a greater extent than at present as they have considerable potential to greatly improve our understanding of the molecular aspects of reproduction both in health and disease.

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Identification of Antihypertensive Peptides Derived from Low Molecular Weight Casein Hydrolysates Generated during Fermentation by Bifidobacterium longum KACC 91563

  • Ha, Go Eun;Chang, Oun Ki;Jo, Su-Mi;Han, Gi-Sung;Park, Beom-Young;Ham, Jun-Sang;Jeong, Seok-Geun
    • Food Science of Animal Resources
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    • v.35 no.6
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    • pp.738-747
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    • 2015
  • Angiotensin-converting enzyme (ACE) inhibitory activity was evaluated for the low-molecular-weight fraction (<3 kDa) obtained from milk fermentation by Bifidobacterium longum KACC91563. The ACE inhibitory activity in this fraction was 62.3%. The peptides generated from the <3 kDa fraction were identified by liquid chromatography-electrospray ionization quantitative time-of-flight mass spectrometry analysis. Of the 28 peptides identified, 11 and 16 were identified as β-casein (CN) and αs1-CN, respectively. One peptide was identified as κ-CN. Three peptides, YQEPVLGPVRGPFPIIV, QEPVLGPVRGPFPIIV, and GPVRGPFPIIV, from β-CN corresponded to known antihypertensive peptides. We also found 15 peptides that were identified as potential antihypertensive peptides because they included a known antihypertensive peptide fragment. These peptides were as follows: RELEELNVPGEIVE (f1-14), YQEPVLGPVRGPFP (f193-206), EPVLGPVRGPFPIIV (f195-206), PVLGPVRGPFPIIV (f196-206), VLGPVRGPFPIIV (f197-206), and LGPVRGPFPIIV (f198-206) for β-CN; and APSFSDIPNPIGSENSEKTTMPLW (f176-199), SFSDIPNPIGSENSEKT- TMPLW (f178-199), FSDIPNPIGSENSEKTTMPLW (f179-199), SDIPNPIGSENSEKTTMPLW (f180-199), DIPNPIGSENSEKTTMPLW (f181-199), IPNPIGSENSEKTTMPLW (f182-199), PIGSENSEKTTMPLW (f185-199), IGSENSEKTTMPLW (f186-199), and SENSEKTTMPLW (f188-199) for αs1-CN. From these results, B. longum could be used as a starter culture in combination with other lactic acid bacteria in the dairy industry, and/or these peptides could be used in functional food manufacturing as additives for the development of a product with beneficial effects for human health.

Prevalence and Microbial Flora of Chicken Slaughtering and Processing Procedure

  • Seol, Kuk-Hwan;Han, Gi-Sung;Kim, Hyoun Wook;Chang, Oun-Ki;Oh, Mi-Hwa;Park, Beom-Young;Ham, Jun-Sang
    • Food Science of Animal Resources
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    • v.32 no.6
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    • pp.763-768
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    • 2012
  • This study has been performed to measure the prevalence and microbial flora on chicken slaughtering as well as the processing process from the months of October to November. Whole-chicken rinsing technique was used in order to analyze the incidence of microorganisms on chicken carcass at the stage before chilling (after evisceration), after chilling and after cutting. The swab technique was used on processing the processed samples, such as working plates and cutting knives. Brine and cooling water from four cooling tubs were taken from each processing processes and were used as samples. Furthermore, the matrix-assisted laser desorption/ionization mass spectrometry (MALDI MS) for whole cell fingerprinting in combination with a dedicated bioinformatic software tool was used to identify the isolated microorganisms. Of the tested samples and processes, brine ($4.50{\pm}0.64$ Log CFU/mL) and chicken carcass before chilling ($4.15{\pm}0.46$ Log CFU/mL) showed the highest population of microorganisms; the predominant microbial flora of them were Moellerella wisconsensis (54.84%), a member of the Enterobacteriaceae family, and Escherichia coli (60.36%), respectively. However, the predominant microbial flora of cut carcass was changed to Staphylococcus aureus (27.32%), which is a kind of pathogenic microorganism that can cause a food-borne illness. Therefore, the slaughtering and processing procedure of chicken are needed to be controlled more hygienically.

Development of photoresist ashing process in an ICP with periodic axial magnetic field (주기적인 축방향 자기장을 추가한 유도결합형 플라즈마 장치에서의 감광제 제거공정 개발)

  • 송호영;라상호;박세근;오범환
    • Proceedings of the IEEK Conference
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    • 2000.06b
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    • pp.290-293
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    • 2000
  • Low frequency(<100Hz) weak magnetic field(<20gauss) is applied axially to an inductively coupled oxygen plasma(ICP), and its plasma characteristics are monitored by OES(Optical Emission Spectroscopy) and Langmuir probe. It is found that periodic magnetic field enhances ashing rate by 25% and improves its uniformity upto 4.5% over 8" wafer. From electron energy distribution function, both low and high energy electrons are identified and relative abundancy is found to be controlled by the applied frequency. Moreover, it is observed that ionization and dissociation species are varied with applied frequency. We insert an aluminium baffle in the chamber to get better uniformity and less plasma damage.

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