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Electrospray Ionization Mass Spectrometric Observation of Oligomers in Paal-Knorr Synthesis of 2,5-Dimethyl-1-phenylpyrrole

  • Park, So-Young;Chun, Man-Seog;Song, Jin-Su;Kim, Hie-Joon
    • Bulletin of the Korean Chemical Society
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    • v.26 no.4
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    • pp.575-578
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    • 2005
  • Electrospray ionization mass spectrometry (ESI MS) was used, along with gas chromatography-mass spectrometry (GC-MS), to monitor Paal-Knorr synthesis of 2,5-dimethyl-1-phenylpyrrole by condensation of aniline with 2,5-hexanedione. In addition to 2,5-dimethyl-1-phenylpyrrole observed as a single spot by TLC, unexpected dimer size compounds were observed by GC-MS. Dimers and trimers were observed by ESI MS. ESI tandem mass spectrometry was used to select plausible structures for the dimer. ESI MS with or without liquid chromatographic separation is useful for observing oligomeric byproducts with low volatility produced in organic reactions.

Structural Analysis of [Cu(II)-amyloidogenic peptide] Complexes

  • Cha, Eugene;Seo, Jae-Hong;Kim, Ho-Tae
    • Mass Spectrometry Letters
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    • v.9 no.1
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    • pp.17-23
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    • 2018
  • Studies on the interactions of amyloidogenic proteins with trace metals, such as copper, have indicated that the metal ions perform a critical function in the early oligomerization process. Herein, we investigate the effects of Cu(II) ions on the active sequence regions of amyloidogenic proteins using electrospray ionization mass spectrometry (ESI-MS) and collision induced dissociation tandem MS (CID-MS/MS). We chose three amyloidogenic peptides NNQQNY, LYQLEN, and VQIVYK from yeast prion like protein Sup35, insulin chain A, and tau protein, respectively. [Cu-peptide] complexes for all three peptides were observed in the mass spectra. The mass spectra also show that increasing Cu(II) concentrations decrease the population of existing peptide oligomers. The tandem mass spectrum of NNQQNY shows preferential binding for the N-terminal region. All three peptides are likely to appear to be in a Cu-monomer-monomer (Cu-M-M) structure instead of a monomer-Cu-monomer (M-Cu-M) structure.

The Study on the Analysis Method of Tetrodotoxin in Puffer Fish (복어 중 테트로도톡신 분석법에 관한 연구)

  • Kang, Young-Woon;Lee, Yoon-Suk;Park, Sung-Kug;Seo, Jung-Heok;Kim, Mee-Hye
    • Journal of Food Hygiene and Safety
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    • v.27 no.1
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    • pp.37-41
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    • 2012
  • The current standard for testing tetrodotoxin (TTX) in foodstuffs is the mouse bioassay (MBA) in Korea as in many other countries. However, this test suffers from potential ethical concerns over the use of live animals. In addition, the mouse bioassay does not test for a specific toxin thus a sample resulting in mouse incapacitation would need further confirmatory testing to determine the exact source toxin (e.g., TTX, STX, brevotoxin, etc.). Furthermore, though the time of death is proportional to toxicity in this assay, the dynamic range for this proportional relationship is small thus many samples must be diluted and new mice be injected to yield a result that falls within the quantitative dynamic range. Therefore, in recent years, there have been many efforts in this field to develop alternative assays. High performance liquid chromatography (HPLC) coupled with mass spectrometry (MS) has been emerged as one of the most promising options. A LC-MS-MS method involves solid-phase extraction (SPE) and followed by analysis using an electrospray in the positive ionization mode and multiple reactions monitoring (MRM). To adopt LC-MS-MS method as alternative standard for testing TTX, we performed a validation study for the quantification of TTX in puffer fish. This LC-MS-MS method showed good sensitivity as limits of detection (LOD) of $0.03{\sim}0.08{\mu}g/g$ and limits of quantification (LOQ) of $0.10{\sim}0.25{\mu}g/g$. The linearity ($r^2$) of tetrodotoxin were 0.9986~0.9997, the recovery were 80.9~103.0% and the relative standard deviations (RSD) were 4.3~13.0%. The correlation coefficient between the mouse bioassay and LC/MS/MS method was higher than 0.95.

A Research of Anomaly Detection Method in MS Office Document (MS 오피스 문서 파일 내 비정상 요소 탐지 기법 연구)

  • Cho, Sung Hye;Lee, Sang Jin
    • KIPS Transactions on Computer and Communication Systems
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    • v.6 no.2
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    • pp.87-94
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    • 2017
  • Microsoft Office is an office suite of applications developed by Microsoft. Recently users with malicious intent customize Office files as a container of the Malware because MS Office is most commonly used word processing program. To attack target system, many of malicious office files using a variety of skills and techniques like macro function, hiding shell code inside unused area, etc. And, people usually use two techniques to detect these kinds of malware. These are Signature-based detection and Sandbox. However, there is some limits to what it can afford because of the increasing complexity of malwares. Therefore, this paper propose methods to detect malicious MS office files in Computer forensics' way. We checked Macros and potential problem area with structural analysis of the MS Office file for this purpose.

Carbohydrate Drug (Acarbose) Analysis using by the On-line HPLC/Electrospray Ionization-Mass Spectrometry (On-line HPLC/ESI-MS를 이용한 탄수화물제제 (Acarbose) 분석연구)

  • Cho, Hyun-Woo;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.15 no.6
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    • pp.574-579
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    • 2002
  • A sensitive and easy high performance liquid chromatograph (HPLC) / electrospray ionization (ESI)-mass spectrometric (MS) method has been developed for the quantitative and qualitative analyses of acarbose and its metabolites. After plasma samples were simply filtered with a syringe filter, the filtered plasma was analyzed by LC/MS. The standard calibration curve for acarbose was linear ($r^2=0.9963$) over the concentration range $0.1{\sim}10{\mu}g/m{\ell}$ in plasma. The metabolite component-I and II, which were metabolized by the ${\alpha}$-amylase and ${\beta}$-amylase, were found also by in vitro incubation. The developed method can be utilized to study acarbose and the other carbohydrates.

320 Pesticides Analysis of Essential Oils by LC-MS/MS and GC-MS/MS (LC-MS/MS 와 GC-MS/MS 를 이용한 에센셜 오일 중 320 종 잔류농약 분석법 개발)

  • Oh, Ka Hyang;Park, Sung Mak;Lee, So Min;Jung, So Young;Kwak, Byeong-Mun;Lee, Mi-Gi;Lee, Mi Ae;Choi, Sung Min;Bin, Bum-Ho
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.47 no.4
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    • pp.317-331
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    • 2021
  • Essential oil is a volatile substance obtained by physically obtaining fragrant plant materials made by one single plant and plant species, and is widely used for cosmetics, fragrances, and aroma therapy due to its excellent preservation, sterilization, and antibacterial effects. When essential oil would undergo the extraction and concentration processes, the agricultural chemicals thereof would be extracted and concentrated only to be harmful to the human body. This study analyzes 320 residual agricultural chemicals concentrated in the essential oil, and to this end, LC-MS/MS and GC-MS/MS are used, while the freezing process is applied instead of the conventional refining process hexane, to improve the preprocessing method. As a result of analyzing the essential oil, such ingredients as chlorpyrifos, piperonyl butoxide and silafluofen have been detected in Basil oil and Clove leaf oil. Hence, it is perceived that the residual agricultural chemicals should continue to be monitored for the essential oil.

Analysis of Myosin Heavy Chain Isoforms from Longissimus Thoracis Muscle of Hanwoo Steer by Electrophoresis and LC-MS/MS

  • Kim, Gap-Don
    • Food Science of Animal Resources
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    • v.34 no.5
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    • pp.656-664
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    • 2014
  • The purpose of this study was to analyze myosin heavy chain (MHC) isoforms in bovine longissimus thoracis (LT) muscle by liquid chromatography (LC) and mass spectrometry (MS). LT muscles taken from Hanwoo (Korean native cattle) steer (n=3) used to separate myosin bands by sodium dodecyl sulfate-polyacrylamide gel electrophoresis. The peptide queries were obtained from the myosin bands by LC-MS/MS analysis following in-gel digestion with trypsin. A total of 33 and 43 queries were identified as common and unique peptides, respectively, of MHC isoforms (individual ions scores >43 indicate identity or extensive homology, p<0.05). MHC-1 (IIx), -2 (IIa), -4 (IIb), and -7 (slow/I) were identified based on the Mowse score (5118, 3951, 2526, and 2541 for MHC-1, -2, -4, and -7, respectively). However, more analysis is needed to confirm the expression of MHC-4 in bovine LT muscle because any query identified as a unique peptide of MHC-4 was not found. The queries that were identified as unique peptides could be used as peptide markers to confirm MHC-1 (14 queries), -2 (8 queries), and -7 (21 queries) in bovine LT muscle; no query identified as a unique peptide of MHC-4 was found. LC-MS/MS analysis is a useful approach to study MHC isoforms at the protein level.

MS64: A Fast Stream Cipher for Mobile Devices (모바일 단말에 적합한 고속 스트림 암호 MS64)

  • Kim, Yoon-Do;Kim, Gil-Ho;Cho, Gyeong-Yeon;Seo, Kyung-Ryong
    • Journal of Korea Multimedia Society
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    • v.14 no.6
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    • pp.759-765
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    • 2011
  • In this paper, we proposed fast stream cipher MS64 for use mobile that it is secure, fast, and easy to implement software. The proposed algorithm use the fast operating 213-bit arithmetic shift register(ASR) to generate a binary sequence and produce 64-bit stream cipher by using simple logical operation in non linear transform. MS64 supports 128-bit key in encryption algorithm and satisfy with the safety requirement in modern encryption algorithm. In simulation result shows that MS64 is faster than a 32-bit stream cipher SSC2 in the speed of operation with small usage of memory thus MS64 can be used for mobile devices with fast ciphering.

Applicability of CCT-ICP-MS for the Determination of Trace Elements in Airborne Particulate Matters (CCT-ICP-MS의 대기분진내 미량원소분석에 대한 적용성)

  • 임종명;이진홍;서만철
    • Journal of Korean Society for Atmospheric Environment
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    • v.20 no.3
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    • pp.397-409
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    • 2004
  • There has been few studies of either domestic or international to apply CCT-ICP-MS for the precise analysis of As and Cr components associated with airborne particulate matter. To date, the use of CCT-ICP-MS is strongly recommended for the accurate analysis of the toxic trace metals; this is because CCT-ICP-MS technique prevents polyatomic spectral interferences involved in the determination of As and/or Cr components. Taking advantage of CCT-ICP-MS technique, the measurements of about 20 metals were undertaken in this study. The standard reference material (NIST SRM 2783) was used for analytical quality control. To improve analytical accuracy and of acid efficiency, we selected nitric acid based on a test of three kinds of acid for microwave digestion method 1 ) nitric acid. 2) nitric acid and hydrogen peroxide. and 3) nitric acid and perchloric acid. When this method was employed, relative errors to SRM values of Al, As, Cr Fe, Mg, Mn, Pb, Sb, V, and Zn fell below 20%, while those or Ca, Si, and Ti were higher than 20%. The overall results of our study show that the concentrations of As and V determined by CCT-ICP-MS were satisfied with the certificated values within a relative error of 20e1c, whereas those determined by ICP-MS were 10 times higher than the certificated values.

Shoot Regeneration from the Leaf Explants of Tetragonia tetragonoides $O.\;K_{UNTZE}$ (번행초의 잎 절편으로부터 신초의 재분화)

  • Hwang, Sung-Jin;Pyo, Byoung-Sik;Hwang, Baik
    • Korean Journal of Medicinal Crop Science
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    • v.10 no.2
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    • pp.116-119
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    • 2002
  • A protocol has been developed for differentiation of adventitious shoots directly from leaf segments of Tetragonia tetragonoides O. Kuntze. Murashige and Skoog (MS) medium supplemented with 2 mg/L $N^6-benzyladenine$ (BA) and 0.5 mg/L ${\alpha}-naphthaleneacetic$ acid (NAA) supported the induction of adventitious shoots from leaf explants. Adventitious shoots were multiplied by subculturing on the double strength MS (2MS) medium supplemented with 0.5 mg/L NAA and 2 mg/L BA. Shoots were rooted on MS basal medium without any growth regulators.