• Title/Summary/Keyword: High-resolution mass spectrometry

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Flavonol Glycosides with Antioxidant Activity from the Aerial Parts of Epimedium koreanum Nakai

  • Kim, Eun-Sil;Kim, Mi-Kyung;Kang, Hyun-Kyu;Park, Young-In;Dong, Mi-Sook;Kim, Dong-Hyun;Chung, Ha-Sook
    • Natural Product Sciences
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    • v.14 no.4
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    • pp.233-238
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    • 2008
  • The aerial parts of Epimedium koreanum Nakai have been used to stimulate hormone secretion in treating impotence. Ten flavonol glycosides, 3,4,5-trihydroxy-8-prenylflavone 7-O-[${\beta}$-D-glucopyranosyl($1{\rightarrow}2$)-${\beta}$-D-glucopyranoside] (1), hyperoside (2), icarisid II (3), 2"-O-Rhamnosylicarisid II (4), epimedin A (5), epimedin B (6), epimedin C (7), icariin (8), hexandraside E (9), and epimedoside A (10) were isolated from the an ethylacetate soluble extracts of the aerial parts of Epimedium koreanum Nakai through activity-monitord fractionation and isolation method. The structures of compounds 1 - 10 were elucidated by high resolution fast atom bombardment mass spectrometry and two dimentional nuclear magnetic resonance spectroscopy analysis. Compounds 1 and 4 showed potent antioxidant activity, with $IC_{50}$ values of 19.7 and 11.5 ${\mu}g$/mL and 88.2 and 90.5 ${\mu}M$, respectively.

Analysis of Zirconium and Nickel Based Alloys and Zirconium Oxides by Relative and Internal Monostandard Neutron Activation Analysis Methods

  • Shinde, Amol D.;Acharya, Raghunath;Reddy, Annareddy V.R.
    • Nuclear Engineering and Technology
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    • v.49 no.3
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    • pp.562-568
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    • 2017
  • Background: The chemical characterization of metallic alloys and oxides is conventionally carried out by wet chemical analytical methods and/or instrumental methods. Instrumental neutron activation analysis (INAA) is capable of analyzing samples nondestructively. As a part of a chemical quality control exercise, Zircaloys 2 and 4, nimonic alloy, and zirconium oxide samples were analyzed by two INAA methods. The samples of alloys and oxides were also analyzed by inductively coupled plasma optical emission spectroscopy (ICP-OES) and direct current Arc OES methods, respectively, for quality assurance purposes. The samples are important in various fields including nuclear technology. Methods: Samples were neutron irradiated using nuclear reactors, and the radioactive assay was carried out using high-resolution gamma-ray spectrometry. Major to trace mass fractions were determined using both relative and internal monostandard (IM) NAA methods as well as OES methods. Results: In the case of alloys, compositional analyses as well as concentrations of some trace elements were determined, whereas in the case of zirconium oxides, six trace elements were determined. For method validation, British Chemical Standard (BCS)-certified reference material 310/1 (a nimonic alloy) was analyzed using both relative INAA and IM-NAA methods. Conclusion: The results showed that IM-NAA and relative INAA methods can be used for nondestructive chemical quality control of alloys and oxide samples.

RK-270D and E, Oxindole Derivatives from Streptomyces sp. with Anti-Angiogenic Activity

  • Jang, Jun-Pil;Jang, Mina;Nogawa, Toshihiko;Takahashi, Shunji;Osada, Hiroyuki;Ahn, Jong Seog;Ko, Sung-Kyun;Jang, Jae-Hyuk
    • Journal of Microbiology and Biotechnology
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    • v.32 no.3
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    • pp.302-306
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    • 2022
  • A chemical investigation of a culture extract from Streptomyces sp. RK85-270 led to the isolation and characterization of two new oxindoles, RK-270D (1) and E (2). The structures of 1 and 2 were determined by analyzing spectroscopic and spectrometric data from 1D and 2D NMR and High-resolution electrospray ionization mass spectrometry (HRESIMS) experiments. Compound 1 exhibited anti-angiogenic activities against human umbilical vein endothelial cells (HUVECs) without cytotoxicity. Results of Western blot analysis revealed that 1 inhibits VEGF-induced angiogenesis in the HUVECs via VEGFR2/ p38 MAPK-mediated pathway.

Evaluation of human exposure to polychlorinated biphenyls using human serum by congener-specific analysis (혈액 중 PCBs 이성질체별 분석에 의한 인체 노출 평가)

  • Park, Hyo-Keun;Lee, Se-Jin;Jin, Guang-Zhu;Kang, Jung-Ho;Baek, Song-E;Chang, Yoon-Seok
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.73-85
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    • 2006
  • Blood serum concentrations of polychlorinated biphenyls (PCBs) were measured in employees who worked at a municipal solid waste incinerator (MSWI), members of residential community who lived near the MSWI (<0.3km) and members of residential community lived far from the MSWI (>10 km). Human blood serum samples were analyzed for all PCB congeners using high-resolution gas chromatography/high-resolution mass spectrometry (HRGC/HRMS). The mean levels of total PCBs and dioxin-like PCBs in 87 serum samples were 242.77 ng/g lipid and 8.83 TEQ pg/g lipid, respectively. The PCB homologue profiles showed that penta-, hexa-, hepta-chlorinated biphenyls contributed more than 80% of the total PCBs concentration. The most abundant congeners were PCB153, PCB138, PCB180, PCB187, PCB118. A statistical analysis was performed to determine whether there were significant correlations between PCB concentrations and specific variables such as age, gender, smoking habits, occupation, BMI (Body Mass Index) and time of residence. As a result, the age was found to be strongly correlated with serum PCB concentrations. In addition, there were strong correlations between total PCBs and PCB153 (r=0.93, p<.0001), dioxin-like PCBs and PCB118 (r=0.98, p<.0001). So these two congeners are satisfactory indicators for total PCB concentrations and dioxin-like PCBs in human blood respectively.

Synthesis and Characterization of Two Different 1,3-Dithiole-2-thiones as the Precursors of TTF Donor Molecule (TTF 주게분자의 전구체로서 두 가지 다른 1,3-Dithiole-2-thione 화합물의 합성 및 특성화)

  • Kim, Young-Youn;Lee, Ha-Jin;Namgoong, Sung Keon;Hong, Jong-Ki;Noh, Dong-Youn
    • Journal of the Korean Chemical Society
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    • v.44 no.6
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    • pp.513-517
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    • 2000
  • As a precursor of tetrathiafulvalene (TTF) derivative, 5,6-dimethyl-1,3-dithiolo[4,5-b][1,4]dithiin-2-thione (compound 3) was synthesized by the unusual Lawesson's reaction. Depending upon the substituents such as dimethyl and diphenyl groups, two different products containing 1,4-dithiin and thiophene moieties, respectively, were obtained and characterized by $^{13}C$ NMR and high-resolution electron impact (HREI) mass spectroscopy. The formation of 3 was further characterized by X-ray structure analysis. Crystallographic data for 3: triclinic, space group P1, a=4.145(2)$\AA$, b=10.600(2)$\AA$, c=12.279(2)$\AA$, $\alpha$=71.440(10)$^{\circ}$, $\beta$=84.30(2)$^{\circ}$, $\gamma$=87.31(2)$^{\circ}$, Z=2 and R(wR$_2$)=0.0559(0.1416). The formation mechanism of two products was suggested and compared each other.

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Proteomic Analysis of the Aging-related Proteins in Human Normal Colon Epithelial Tissue

  • Li, Ming;Xiao, Zhi-Qiang;Chen, Zhu-Chu;Li, Jian-Ling;Li, Cui;Zhang, Peng-Fei;Li, Mao-Yu
    • BMB Reports
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    • v.40 no.1
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    • pp.72-81
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    • 2007
  • In order to screen the aging related proteins in human normal colon epithelia, the comparative proteomics analysis was applied to get the two-dimensional electrophoresis (2-DE) profiles with high resolution and reproducibility from normal colon epithelial tissues of young and aged people. Differential proteins between the colon epithelia of two age groups were found with PDQuest software. The thirty five differential protein-spots were identified by peptide mass fingerprint (PMF) based on matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) and database searching. Among them there are sixteen proteins which are significantly up-regulated in the colonic mucosal epithelia of young people group, which include ATP synthase beta chain, electron transfer flavoprotein alpha-subunit, catalase, glutathione peroxidase 1, annexin A2 and heat shock cognate 71 kDa protein, etc.; There are nineteen proteins which are significantly up-regulated in the colonic mucosal epithelia of aged people group, which include far upstream element-binding protein 1, nucleoside diphosphate kinase B, protein disulfide-isomerase precursor and VDAC-2, etc.. The identified differential proteins appear to be involved in metabolism, energy generation, chaperone, antioxidation, signal transduction, protein folding and apoptosis. The data will help to understand the molecular mechanisms of human colon epithelial aging.

Comparative Proteomic Analysis of Yak Follicular Fluid during Estrus

  • Guo, Xian;Pei, Jie;Ding, Xuezhi;Chu, Min;Bao, Pengjia;Wu, Xiaoyun;Liang, Chunnian;Yan, Ping
    • Asian-Australasian Journal of Animal Sciences
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    • v.29 no.9
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    • pp.1239-1246
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    • 2016
  • The breeding of yaks is highly seasonal, there are many crucial proteins involved in the reproduction control program, especially in follicular development. In order to isolate differential proteins between mature and immature follicular fluid (FF) of yak, the FF from yak follicles with different sizes were sampled respectively, and two-dimensional gel electrophoresis (2-DE) of the proteins was carried out. After silver staining, the Image Master 2D platinum software was used for protein analysis and matrix-assisted laser desorption ionization time of flight mass spectrometry (MALDI-TOF-MS) was performed for differential protein identification. The expression level of transferrin and enolase superfamily member 1 (ENOSF1) was determined by Western blotting for verification analysis. The results showed that 2-DE obtained an electrophoresis map of proteins from mature and immature yak FF with high resolution and repeatability. A comparison of protein profiles identified 12 differently expressed proteins, out of which 10 of them were upregulated while 2 were downregulated. Western blotting showed that the expression of transferrin and ENOSF1 was enhanced with follicular development. Both the obtained protein profiles and the differently expressed proteins identified in this study provided experimental data related to follicular development during yak breeding seasons. This study also laid the foundation for understanding the microenvironment during oocyte development.

Anti-Termite Activity of Azadirachta excelsa Seed Kernel and Its Isolated Compound against Coptotermes curvignathus

  • Morina ADFA;Khafit WIRADIMAFAN;Ricky Febri PRATAMA;Angga SANJAYA;Deni Agus TRIAWAN;Salprima YUDHA S.;Masayuki NINOMIYA;Mohamad RAFI;Mamoru KOKETSU
    • Journal of the Korean Wood Science and Technology
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    • v.51 no.3
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    • pp.157-172
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    • 2023
  • Azadirachta excelsa, is a plant belonging to the same genus as Indian neem (Azadirachta indica), and its use as a pesticide is reported by few studies. Despite being a different species, it is expected to have the same biopesticide potential as A. indica. Therefore, this study aims to investigate the anti-termite activity of n-hexane and methanol extracts of A. excelsa seed kernel at various concentrations against Coptotermes curvignathus. The methanol extract demonstrated greater termicidal activity than n-hexane at doses test of 2%, 4%, and 8%. It also showed 100% termite mortality on the third day of administering the 8% dose. According to the gas chromatography with mass spectrometry data, the putative main components of the n-hexane extract were hexadecanoic acid, ethyl ester (18.99%), 9,12-octadecadienoic acid (Z,Z)- (16.31%), and 9-octadecenal (16.23%). In contrast, the principal constituents of methanol extract were patchouli alcohol (28.1%), delta-guaiene (15.15%), and alpha-guaiene (11.93%). Furthermore, limonoids profiling of A. excelsa methanol extract was determined using Ultrahigh-performance liquid chromatography coupled with quadrupole-Orbitrap high-resolution mass spectrometry. The number of limonoids identified tentatively was fifteen, such as 6-deacetylnimbin, nimbolidin C, nimbolide, 6-acetylnimbandiol, 6-deacetyl-nimbinene, salannol, 28-deoxonimbolide, gedunin, nimbandiol, epoxyazadiradione, azadirone, 2',3'-dihydrosalannin, marrangin, nimbocinol, and azadirachtin. They were the same as those reported in the seed and leaves of A. indica, but its largest component in A. excelsa was 6-deacetylnimbin. As a result, the presence of these compounds may be responsible for the anti-termite activity of A. excelsa seed kernel extract. Additionally, column chromatography of methanol extract yielded 6-deacetylnimbin, which was found to be antifeedant and termiticide against C. curvignathus.

Effect of Disk Rotational Speed on Contamination Nano Particles Generated in a Hard Disk Drive (하드 디스크 드라이브 회전수 변화가 드라이브 내 나노 오염 입자 발생에 미치는 영향)

  • Lee, Dae-Young;Hwang, Jung-Ho;Bae, Gwi-Nam
    • Transactions of the Korean Society of Mechanical Engineers B
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    • v.28 no.8 s.227
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    • pp.976-983
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    • 2004
  • In high-density hard disk drives, the slider should be made to fly close to the magnetic recording disk to generate better signal resolution and at an increasingly high velocity to achieve better data rate. The slider disk interaction in CSS (contact-start-stop) mode is an important source of particle generation. Contamination particles in the hard disk drive can cause serious problems including slider crash and thermal asperities. We investigated the number and the sizes of particles generated in the hard disk drive, operating at increasing disk rotational speeds, in the CSS mode. CNC (condensation nucleus counter) and PSS (particle size selector) were used for this investigation. In addition, we examined the particle components by using SEM (scanning electron microscopes), AES (auger electron spectroscopy), and TOF-SIMS (time of flight-secondary ions mass spectrometry). The increasing disk rotational speed directly affected the particle generation by slider disk interaction. The number of particles that were generated increased with the disk rotational speed. The particle generation rate increased rapidly at motor speeds above 8000 rpm. This increase may be due to the increased slider disk interaction. Particle sizes ranged from 14 to 200 nm. The particles generated by slider disk interaction came from the lubricant on the disk, coating layer of the disk, and also slider surface.

Analysis of polychlorinated dibenzo-p-dioxins and dibenzofurans to assure safety of imported meat (수입 식육의 안전성 확보를 위한 polychlorinated dibenzo-p-dioxins와 dibenzofurans 분석)

  • Kim, MeeKyung;Kim, Dong-Gyu;Kim, Sooyeon;Choi, Si-Weon;Kwon, Jin-Wook;Yun, Seon Jong;Song, Sung Ok;Chung, Gab Soo
    • Korean Journal of Veterinary Research
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    • v.48 no.1
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    • pp.39-48
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    • 2008
  • Polychlorinated dibenzo-p-dioxins (PCDDs) and dibenzofurans (PCDFs) are ubiquitous and can contaminate the food chain. A study monitoring PCDD/Fs in imported meat was conducted at the National Veterinary Research and Quarantine Service (NVRQS, Republic of Korea) in order to maintain food safety from the bioaccumulative PCDD/Fs. Seventeen PCDD/Fs with toxic equivalency factors (TEFs) established by World Health Organization (WHO, 1998) were analyzed in imported beef, pork, and chicken by high resolution gas chromatography/mass spectrometry (HR-GC/MS). Results of the monitoring for the last 5 years are presented. The levels of PCDD/Fs were similar to other studies except two unusually high concentrations in pork and beef. Excessive levels greater than the Korean provisional maximum residue limit of PCDD/Fs were found in a sample of pork imported from Chile and a sample of beef imported from U.S, and those products were rejected and returned. There was no obvious trend or differences with respect to time or origin of meat in this study.